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Sample records for drop microextraction combined

  1. Stepwise injection potentiometric determination of caffeine in saliva using single-drop microextraction combined with solvent exchange.

    Science.gov (United States)

    Timofeeva, I; Medinskaia, K; Nikolaeva, L; Kirsanov, D; Bulatov, A

    2016-04-01

    A flow potentiometric method for determination of caffeine in saliva is suggested. This task is important for non-invasive assessment of drug metabolizing system activity in hepatocytes. In the current study, stepwise injection analysis (SWIA) was successfully combined with single-drop liquid microextraction (SDLME) and solvent exchange procedure. The method is based on the caffeine SDLME with subsequent solvent evaporation and dissolution of analyte in sulfuric acid followed by potentiometric detection using poly(vinyl chloride) membrane electrode containing potassium tetrakis[3,5-bis(trifluoromethyl)phenyl]borate as electroactive component. SDLME was employed for elimination of interfering matrix effects of saliva and caffeine metabolites such as theophylline, theobromine and paraxanthine. A linear range of 10(-5)-10(-2)M was established for caffeine with detection limit at 6 × 10(-6)M. The sample throughput was 6 samples h(-1). The proposed method was successfully applied to the determination of caffeine in saliva and the analytical results agreed well with the results obtained with reference HPLC method. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. Low-density solvent-based dispersive liquid-liquid microextraction combined with single-drop microextraction for the fast determination of chlorophenols in environmental water samples by high performance liquid chromatography-ultraviolet detection.

    Science.gov (United States)

    Li, Xiaoyi; Xue, Aifang; Chen, Hao; Li, Shengqing

    2013-03-08

    A new format of fast three-phase microextraction by combining low-density solvent-based dispersive liquid-liquid microextraction (DLLME) and single-drop microextraction (SDME) was for the first time developed for the determination of chlorophenols in environmental water samples. The extraction procedure includes a 2 min DLLME pre-extraction and a 10 min SDME back-extraction. A portion of low-density solvent (toluene) was used as organic phase and injected into the aqueous sample (donor phase) with methanol as disperser. The analytes were pre-extracted into the organic phase within 2 min. A thin layer of the organic phase formed on the top of the aqueous phase by a 2 min centrifugation. Then a drop of acceptor solution was introduced into the upper layer and SDME was carried out for the back-extraction. The stirring step typically involved in SDME and LLLME is avoided with the benefit of the high speed and efficiency of DLLME pre-extraction. After extraction, the acceptor drop was withdrawn and directly injected into a high performance liquid chromatography instrument with ultraviolet detection for analysis. Five chlorophenols, 4-chlorophenol, 2-chlorophenol, 2,4-dichlorophenol, 2,4,6-trichlorophenol, and pentachlorophenol, were selected as model compounds for developing and evaluating the method. Factors affecting extraction efficiency were studied, including the organic solvent, the disperser solvent, the composition of donor phase and acceptor phase, the volume of acceptor microdrop, and the extraction time. At optimal conditions, the method showed low detection limit (0.016-0.084 μg/L) for the five chlorophenols, good linearity (from 0.2-250 to 1.0-250 μg/L, depending on the analytes) and repeatability (RSD below 8.2, n=5). The simple, fast, and efficient feature of the proposed method was demonstrated by the analysis of chlorophenols in environmental water samples. Copyright © 2013 Elsevier B.V. All rights reserved.

  3. Optimization of dispersive liquid-phase microextraction based on solidified floating organic drop combined with high-performance liquid chromatography for the analysis of glucocorticoid residues in food.

    Science.gov (United States)

    Huang, Yuan; Zheng, Zhiqun; Huang, Liying; Yao, Hong; Wu, Xiao Shan; Li, Shaoguang; Lin, Dandan

    2017-05-10

    A rapid, simple, cost-effective dispersive liquid-phase microextraction based on solidified floating organic drop (SFOD-LPME) was developed in this study. Along with high-performance liquid chromatography, we used the developed approach to determine and enrich trace amounts of four glucocorticoids, namely, prednisone, betamethasone, dexamethasone, and cortisone acetate, in animal-derived food. We also investigated and optimized several important parameters that influenced the extraction efficiency of SFOD-LPME. These parameters include the extractant species, volumes of extraction and dispersant solvents, sodium chloride addition, sample pH, extraction time and temperature, and stirring rate. Under optimum experimental conditions, the calibration graph exhibited linearity over the range of 1.2-200.0ng/ml for the four analytes, with a reasonable linearity(r 2 : 0.9990-0.9999). The enrichment factor was 142-276, and the detection limits was 0.39-0.46ng/ml (0.078-0.23μg/kg). This method was successfully applied to analyze actual food samples, and good spiked recoveries of over 81.5%-114.3% were obtained. Copyright © 2017. Published by Elsevier B.V.

  4. Headspace liquid-phase microextraction of methamphetamine and amphetamine in urine by an aqueous drop

    International Nuclear Information System (INIS)

    He Yi; Vargas, Angelica; Kang, Youn-Jung

    2007-01-01

    This study developed a headspace liquid-phase microextraction (LPME) method by using a single aqueous drop in combination with high performance liquid chromatography (HPLC)-UV detection for the determination of methamphetamine (MAP) and amphetamine (AP) in urine samples. The analytes, volatile and basic, were released from sample matrix into the headspace first, and then protonated and dissolved in an aqueous H 3 PO 4 drop hanging in the headspace by a HPLC syringe. After extraction, this drop was directly injected into HPLC. Parameters affecting extraction efficiency were investigated and optimized. This method showed good linearity in the investigated concentration range of 1.0-1500 μg L -1 , repeatability of the extraction (R.S.D. -1 for both analytes). Enrichment factors of about 400-fold and 220-fold were achieved for MAP and AP, respectively, at optimum conditions. The feasibility of the method was demonstrated by analyzing human urine samples

  5. Headspace single drop microextraction versus dispersive liquid-liquid microextraction using magnetic ionic liquid extraction solvents.

    Science.gov (United States)

    An, Jiwoo; Rahn, Kira L; Anderson, Jared L

    2017-05-15

    A headspace single drop microextraction (HS-SDME) method and a dispersive liquid-liquid microextraction (DLLME) method were developed using two tetrachloromanganate ([MnCl 4 2- ])-based magnetic ionic liquids (MIL) as extraction solvents for the determination of twelve aromatic compounds, including four polyaromatic hydrocarbons, by reversed phase high-performance liquid chromatography (HPLC). The analytical performance of the developed HS-SDME method was compared to the DLLME approach employing the same MILs. In the HS-SDME approach, the magnetic field generated by the magnet was exploited to suspend the MIL solvent from the tip of a rod magnet. The utilization of MILs in HS-SDME resulted in a highly stable microdroplet under elevated temperatures and long extraction times, overcoming a common challenge encountered in traditional SDME approaches of droplet instability. The low UV absorbance of the [MnCl 4 2- ]-based MILs permitted direct analysis of the analyte enriched extraction solvent by HPLC. In HS-SDME, the effects of ionic strength of the sample solution, temperature of the extraction system, extraction time, stir rate, and headspace volume on extraction efficiencies were examined. Coefficients of determination (R 2 ) ranged from 0.994 to 0.999 and limits of detection (LODs) varied from 0.04 to 1.0μgL -1 with relative recoveries from lake water ranging from 70.2% to 109.6%. For the DLLME method, parameters including disperser solvent type and volume, ionic strength of the sample solution, mass of extraction solvent, and extraction time were studied and optimized. Coefficients of determination for the DLLME method varied from 0.997 to 0.999 with LODs ranging from 0.05 to 1.0μgL -1 . Relative recoveries from lake water samples ranged from 68.7% to 104.5%. Overall, the DLLME approach permitted faster extraction times and higher enrichment factors for analytes with low vapor pressure whereas the HS-SDME approach exhibited better extraction efficiencies for

  6. Headspace single-drop microextraction coupled to microvolume UV-vis spectrophotometry for iodine determination

    International Nuclear Information System (INIS)

    Pena-Pereira, Francisco; Lavilla, Isela; Bendicho, Carlos

    2009-01-01

    Headspace single-drop microextraction has been combined with microvolume UV-vis spectrophotometry for iodine determination. Matrix separation and preconcentration of iodide following in situ volatile iodine generation and extraction into a microdrop of N,N'-dimethylformamide is performed. An exhaustive characterization of the microextraction system and the experimental variables affecting iodine generation from iodide was carried out. The procedure employed consisted of exposing 2.5 μL of N,N'-dimethylformamide to the headspace of a 10 mL acidic (H 2 SO 4 2 mol L -1 ) aqueous solution containing 1.7 mol L -1 Na 2 SO 4 for 7 min. Addition of 1 mL of H 2 O 2 1 mol L -1 for in situ iodine generation was performed. The limit of detection was determined as 0.69 μg L -1 . The repeatability, expressed as relative standard deviation, was 4.7% (n = 6). The calibration working range was from 5 to 200 μg L -1 (r 2 = 0.9991). The large preconcentration factor obtained, ca. 623 in only 7 min, compensate for the 10-fold loss in sensitivity caused by the decreased optical path, which results in improved detection limits as compared to spectrophotometric measurements carried out with conventional sample cells. The method was successfully applied to the determination of iodine in water, pharmaceutical and food samples

  7. Headspace liquid-phase microextraction of methamphetamine and amphetamine in urine by an aqueous drop

    Energy Technology Data Exchange (ETDEWEB)

    He Yi [Department of Sciences, John Jay College of Criminal Justice, City University of New York, 445 W 59th Street, New York, NY 10019 (United States)]. E-mail: yhe@jjay.cuny.edu; Vargas, Angelica [Department of Sciences, John Jay College of Criminal Justice, City University of New York, 445 W 59th Street, New York, NY 10019 (United States); Kang, Youn-Jung [Department of Sciences, John Jay College of Criminal Justice, City University of New York, 445 W 59th Street, New York, NY 10019 (United States)

    2007-04-25

    This study developed a headspace liquid-phase microextraction (LPME) method by using a single aqueous drop in combination with high performance liquid chromatography (HPLC)-UV detection for the determination of methamphetamine (MAP) and amphetamine (AP) in urine samples. The analytes, volatile and basic, were released from sample matrix into the headspace first, and then protonated and dissolved in an aqueous H{sub 3}PO{sub 4} drop hanging in the headspace by a HPLC syringe. After extraction, this drop was directly injected into HPLC. Parameters affecting extraction efficiency were investigated and optimized. This method showed good linearity in the investigated concentration range of 1.0-1500 {mu}g L{sup -1}, repeatability of the extraction (R.S.D. < 5%, n = 6), and low detection limits (0.3 {mu}g L{sup -1} for both analytes). Enrichment factors of about 400-fold and 220-fold were achieved for MAP and AP, respectively, at optimum conditions. The feasibility of the method was demonstrated by analyzing human urine samples.

  8. A simple and rapid dispersive liquid-liquid microextraction based on solidification of floating organic drop method combined with flame atomic absorption spectrometry for preconcentration and determination of copper.

    Science.gov (United States)

    Mirzaei, Mohammad; Behzadi, Mansoureh

    2013-01-01

    A simple and rapid dispersive liquid-liquid microextraction based on solidification of floating organic drop method prior to flame atomic absorption spectrometry was developed for preconcentration and determination of copper. In this technique, simultaneous complex formation and extraction was performed with rapid injection of a mixture containing ethanol, 1-undecanol, and 1-(2-pyridylazo)-2-naphthol into a water sample spiked with Cu(II). After centrifugation, the test tube was cooled in an ice bath, and solidified extract transferred into a conical vial. Finally, it was dissolved into ethanol and copper concentration was determined. Some effective parameters of extraction and complex formation, such as extraction and disperser solvent type and volume, pH, concentration of the chelating agent, salt effect, and extraction time, were optimized. Under the optimum conditions, the calibration graph was linear in the range of 0.50 ng/mL to 0.30 microg/mL, with an LOD of 0.16 ng/mL. The RSD for 10 replicate measurements of 50.0 ng/mL of copper was +/- 1.4%. Two certified reference materials were analyzed, and the determined values were in good agreement with the certified values.

  9. Speciation of As(III) and As(V) in water samples by graphite furnace atomic absorption spectrometry after solid phase extraction combined with dispersive liquid-liquid microextraction based on the solidification of floating organic drop.

    Science.gov (United States)

    Shamsipur, Mojtaba; Fattahi, Nazir; Assadi, Yaghoub; Sadeghi, Marzieh; Sharafi, Kiomars

    2014-12-01

    A solid phase extraction (SPE) coupled with dispersive liquid-liquid microextraction based on the solidification of floating organic drop (DLLME-SFO) method, using diethyldithiphosphate (DDTP) as a proper chelating agent, has been developed as an ultra preconcentration technique for the determination of inorganic arsenic in water samples prior to graphite furnace atomic absorption spectrometry (GFAAS). Variables affecting the performance of both steps were thoroughly investigated. Under optimized conditions, 100mL of As(ΙΙΙ) solution was first concentrated using a solid phase sorbent. The extract was collected in 2.0 mL of acetone and 60.0 µL of 1-undecanol was added into the collecting solvent. The mixture was then injected rapidly into 5.0 mL of pure water for further DLLME-SFO. Total inorganic As(III, V) was extracted similarly after reduction of As(V) to As(III) with potassium iodide and sodium thiosulfate and As(V) concentration was calculated by difference. A mixture of Pd(NO3)2 and Mg(NO3)2 was used as a chemical modifier in GFAAS. The analytical characteristics of the method were determined. The calibration graph was linear in the rage of 10-100 ng L(-1) with detection limit of 2.5 ng L(-1). Repeatability (intra-day) and reproducibility (inter-day) of method based on seven replicate measurements of 80 ng L(-1) of As(ΙΙΙ) were 6.8% and 7.5%, respectively. The method was successfully applied to speciation of As(III), As(V) and determination of the total amount of As in water samples and in a certified reference material (NIST RSM 1643e). Copyright © 2014 Elsevier B.V. All rights reserved.

  10. Single-drop liquid phase microextraction accelerated by surface acoustic wave.

    Science.gov (United States)

    Zhang, Anliang; Zha, Yan

    2013-03-01

    A single-drop liquid phase microextraction method is presented, in which surface acoustic wave (SAW) is used for accelerating extraction speed. A pair of interdigital transducers with 27.5 MHz center frequency is fabricated on a 128° yx-LiNbO3 substrate. A radio frequency signal is applied to one of interdigital transducers to excite SAW. Plastic straw is filled with PDMS, leaving 1 mL for holding sample solution. Plastic straw with sample solution droplet is then dipping into extractant, into which SAW is radiated. Mass transportation from sample solution to extractant drop is accelerated due to acoustic streaming, and extraction time is decreased. An ionic liquid and an acid green-25 solution are used for extraction experiments. Results show that the extraction process is almost finished within 2 min, and extraction speed is increased with radio frequency signal power. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Drop-to-drop solvent microextraction coupled with gas chromatography/mass spectrometry for rapid determination of trimeprazine in urine and blood of rats: application to pharmacokinetic studies.

    Science.gov (United States)

    Agrawal, Kavita; Wu, Hui-Fen

    2007-01-01

    A simple and rapid method based on drop-to-drop solvent microextraction (DDSME) coupled with gas chromatography/mass spectrometry (GC/MS) has been successfully applied for the pharmacokinetic studies of trimeprazine in 8 microL of urine and blood samples of rats. Several factors that influenced the extraction efficiency of DDSME, such as selection of organic solvent, extraction time, exposure volume of organic phase, addition of salt and pH, were optimized. Linearity was obtained over the concentration ranges of 0.2-10, 0.25-7.0 and 0.5-6.0 microg/mL with correlation coefficients of 0.998, 0.996 and 0.993 in deionized water, urine and blood samples of rats, respectively. The limits of detection (LODs) of trimeprazine were 0.05, 0.06 and 0.1 microg/mL in deionized water, urine and blood samples. The concentrations of trimeprazine obtained in urine and blood samples of rats were 0.21-1.25 and 2.72-0.22 microg/mL, respectively, after a single intravenous administration of this drug. The enrichment factors and LOD values obtained by DDSME coupled to GC/MS were compared with those of hollow fiber liquid-phase microextraction (HF-LPME) combined with GC/MS. We believe that this novel approach can be very useful in clinical application since only one microdrop of biological samples was required to perform the pharmacokinetic studies from rats, so the sample pretreatments for animal experiments can be very easy too. Copyright (c) 2007 John Wiley & Sons, Ltd.

  12. Sensitive determination of cadmium using solidified floating organic drop microextraction-slotted quartz tube-flame atomic absorption spectroscopy.

    Science.gov (United States)

    Akkaya, Erhan; Chormey, Dotse Selali; Bakırdere, Sezgin

    2017-09-20

    In this study, solidified floating organic drop microextraction (SFODME) by 1-undecanol was combined with slotted quartz tube flame atomic absorption spectrometry (SQT-FAAS) for the determination of cadmium at trace levels. Formation of a complex with 4,4'-dimethyl-2,2'-bipyridine facilitated the extraction of cadmium from aqueous solutions. Several chemical variables were optimized in order to obtain high extraction outputs. Parameters such as concentration of the ligand, pH, and amount of buffer solution were optimized to enhance the formation of cadmium complex. The SFODME method was assisted by dispersion of extractor solvent into aqueous solutions using 2-propanol. Under the optimum extraction and instrumental conditions, the limit of detection and limit of quantitation values obtained for cadmium using the combined methods (SFODME-SQT-FAAS) were found to be 0.4 and 1.3 μg L -1 , respectively. Matrix effects on the method were also examined for tap water and wastewater, and spiked recovery results were found to be very satisfactory. Graphical Abstract SFODME-SQT-FAAS system for sensitive determination of cadmium.

  13. Sensitive determination of mercury by a miniaturized spectrophotometer after in situ single-drop microextraction.

    Science.gov (United States)

    Yang, Fangwen; Liu, Rui; Tan, Zhiqiang; Wen, Xiaodong; Zheng, Chengbin; Lv, Yi

    2010-11-15

    An in situ single-drop microextraction (SDME) method was developed for trace mercury determination by a miniaturized spectrophotometer, in which a simple and cheap light-emitting diode (LED) was employed as the light source, and a handheld charge coupled device (CCD) was served as the detector. A droplet of 0.006% dithizone-CCl(4) (m/v) was used as extraction phase and hanged on a rolled PTFE tube. LED light was adjusted carefully to pass through the centre of the droplet and the entrance slit of the CCD detector. The radiation intensities of 475 nm before and after SDME (I(0) and I(i)) were recorded for quantification. Under the optimum conditions, the system provided a linear range of 2-50 μg L(-1), with a correlation coefficient of 0.9983 and a limit of detection (3σ) of 0.2 μg L(-1). The enrichment factor was about 69. The present method showed the merits of high sensitivity, simplicity, rapidity, low reagent consumption and field analysis potential. Finally, this method was successfully applied for the determination of the total mercury in spiked tap water sample, spiked river water sample and certified reference material (GBW (E) 080393, simulated water). Copyright © 2010 Elsevier B.V. All rights reserved.

  14. Sensitive determination of mercury by a miniaturized spectrophotometer after in situ single-drop microextraction

    International Nuclear Information System (INIS)

    Yang Fangwen; Liu Rui; Tan Zhiqiang; Wen Xiaodong; Zheng Chengbin; Lv Yi

    2010-01-01

    An in situ single-drop microextraction (SDME) method was developed for trace mercury determination by a miniaturized spectrophotometer, in which a simple and cheap light-emitting diode (LED) was employed as the light source, and a handheld charge coupled device (CCD) was served as the detector. A droplet of 0.006% dithizone-CCl 4 (m/v) was used as extraction phase and hanged on a rolled PTFE tube. LED light was adjusted carefully to pass through the centre of the droplet and the entrance slit of the CCD detector. The radiation intensities of 475 nm before and after SDME (I 0 and I i ) were recorded for quantification. Under the optimum conditions, the system provided a linear range of 2-50 μg L -1 , with a correlation coefficient of 0.9983 and a limit of detection (3σ) of 0.2 μg L -1 . The enrichment factor was about 69. The present method showed the merits of high sensitivity, simplicity, rapidity, low reagent consumption and field analysis potential. Finally, this method was successfully applied for the determination of the total mercury in spiked tap water sample, spiked river water sample and certified reference material (GBW (E) 080393, simulated water).

  15. Speciation and determination of inorganic mercury and methylmercury by headspace single drop microextraction and electrothermal atomic absorption spectrometry in water and fish

    Energy Technology Data Exchange (ETDEWEB)

    Sarica, Deniz Yurtsever [Scientific and Technological Research Council of Turkey, Ankara Test and Analysis Laboratory, TUeBITAK/ATAL, Besevler, Ankara (Turkey); Tuerker, Ali Rehber [Science Faculty, Department of Chemistry, Gazi University, Ankara (Turkey)

    2012-05-15

    In this study, headspace single drop microextraction (HS-SDME) method in combination with electrothermal atomic absorption spectrometry (ETAAS) method was developed and validated for the speciation and determination of inorganic mercury (iHg) and methylmercury (MeHg). MeHg and iHg species were reduced to volatile methylmercury hydride (CH{sub 3}HgH) and elemental mercury, respectively, in the presence of NaBH{sub 4} and trapped onto a drop of acceptor phase in the tip of a microsyringe. Thiourea and ammonium pyrrolydinedithiocarbamate (APDC) were tested as the acceptor phase. The experimental parameters of the method such as microextraction time, temperature, NaBH{sub 4} concentration, acceptor phase concentration, and pH of the medium were investigated to obtain distinctive conditions for mercury species. Possible interference effects have also been investigated. In order to validation of the method, analytical figures of merits such as accuracy, precision, limit of detection (LOD), limit of quantitation (LOQ), and linear working range have been evaluated. Accuracy of the method has been verified by analyzing certified reference materials (BCR 453 Tuna fish) and spiked samples. The proposed method was applied for the speciation and determination of mercury species in water and fish samples. Mercury species (MeHg and iHg) have been determined in the real samples with a relative error less than 10%. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  16. Optimization of a single-drop microextraction method for multielemental determination by electrothermal vaporization inductively coupled plasma mass spectrometry following in situ vapor generation

    International Nuclear Information System (INIS)

    Gil, Sandra; Loos-Vollebregt, Margaretha T.C. de; Bendicho, Carlos

    2009-01-01

    A headspace single-drop microextraction (HS-SDME) method has been developed in combination with electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS) for the simultaneous determination of As, Sb, Bi, Pb, Sn and Hg in aqueous solutions. Vapor generation is carried out in a 40 mL volume closed-vial containing a solution with the target analytes in hydrochloric acid and potassium ferricyanide medium. Hydrides (As, Sb, Bi, Pb, Sn) and Hg vapor are trapped onto an aqueous single drop (3 μL volume) containing Pd(II), followed by the subsequent injection in the ETV. Experimental variables such as medium composition, sodium tetrahydroborate (III) volume and concentration, stirring rate, extraction time, sample volume, ascorbic acid concentration and palladium amount in the drop were fully optimized. The limits of detection (LOD) (3σ criterion) of the proposed method for As, Sb, Bi, Pb, Sn and Hg were 0.2, 0.04, 0.01, 0.07, 0.09 and 0.8 μg/L, respectively. Enrichment factors of 9, 85, 138, 130, 37 and 72 for As, Sb, Bi, Pb, Sn and Hg, respectively, were achieved in 210 s. The relative standard deviations (N = 5) ranged from 4 to 8%. The proposed HS-SDME-ETV-ICP-MS method has been applied for the determination of As, Sb, Bi, Pb, Sn and Hg in NWRI TM-28.3 certified reference material.

  17. Preconcentration of thallium (I) by single drop microextraction with electrothermal atomic absorption spectroscopy detection using dicyclohexano-18-crown-6 as extractant system

    International Nuclear Information System (INIS)

    Chamsaz, Mahmoud; Arbab-Zavar, Mohammad Hossien; Darroudi, Abolfazl; Salehi, Thiery

    2009-01-01

    A simple single drop liquid-phase microextraction (SDME) technique, combined with electrothermal atomic absorption spectroscopy (ETAAS) is developed both to preconcentrate and determine thallium (I) ions in aqueous solutions. The ions were transferred from 10.0 ml of aqueous sample (donor phase) containing 0.5 ml of 1% picric acid as the ion-pair agent into a 3 μl microdrop of nitrobenzene (acceptor phase) containing dicyclohexano-18-crown-6 as the complexing agent. The latter will help to improve the extraction efficiency of the analyte. After the ions have been extracted, the acceptor drop was directly injected into a graphite furnace for thallium (I) determination. Several parameters such as the extracting solvent, extraction time, temperature, concentration of picric acid and crown ether, drop volume and stirring rate were examined. Under the optimized experimental conditions, the detection limit (L.O.D.) was 0.7 ng ml -1 . The relative standard deviation for five replicate analysis of 10 ng ml -1 of thallium (I) was 5.1%. The calibration curve was linear in the range of 3-22 ng ml -1 . The results for determination of thallium in reference material, spiked tap water and seawater demonstrated the accuracy, recovery and applicability of the presented method. The enrichment factor was 50.

  18. Preconcentration of thallium (I) by single drop microextraction with electrothermal atomic absorption spectroscopy detection using dicyclohexano-18-crown-6 as extractant system.

    Science.gov (United States)

    Chamsaz, Mahmoud; Arbab-Zavar, Mohammad Hossien; Darroudi, Abolfazl; Salehi, Thiery

    2009-08-15

    A simple single drop liquid-phase microextraction (SDME) technique, combined with electrothermal atomic absorption spectroscopy (ETAAS) is developed both to preconcentrate and determine thallium (I) ions in aqueous solutions. The ions were transferred from 10.0 ml of aqueous sample (donor phase) containing 0.5 ml of 1% picric acid as the ion-pair agent into a 3 microl microdrop of nitrobenzene (acceptor phase) containing dicyclohexano-18-crown-6 as the complexing agent. The latter will help to improve the extraction efficiency of the analyte. After the ions have been extracted, the acceptor drop was directly injected into a graphite furnace for thallium (I) determination. Several parameters such as the extracting solvent, extraction time, temperature, concentration of picric acid and crown ether, drop volume and stirring rate were examined. Under the optimized experimental conditions, the detection limit (L.O.D.) was 0.7 ng ml(-1). The relative standard deviation for five replicate analysis of 10 ng ml(-1) of thallium (I) was 5.1%. The calibration curve was linear in the range of 3-22 ng ml(-1). The results for determination of thallium in reference material, spiked tap water and seawater demonstrated the accuracy, recovery and applicability of the presented method. The enrichment factor was 50.

  19. Headspace Hanging Drop Liquid Phase Microextraction and Gas Chromatography-Mass Spectrometry for the Analysis of Flavors from Clove Buds

    Energy Technology Data Exchange (ETDEWEB)

    Jung, Mi Jin; Shin, Yeon Jae; Oh, Se Yeon; Kim, Nam Sun; Kim, Kun; Lee, Dong Sun [Seoul Women' s University, Seoul (Korea, Republic of)

    2006-02-15

    A novel sample pretreatment technique, headspace hanging drop liquid phase microextraction (HS-LPME) was studied and applied to the determination of flavors from solid clove buds by gas chromatography-mass spectrometry (GC-MS). Several parameters affecting on HS-LPME such as organic solvent drop volume, extraction time, extraction temperature and phase ratio were investigated. 1-Octanol was selected as the extracting solvent, drop size was fixed to 0.6 μL. 60 min extraction time at 25 .deg. C was chosen. HS-LPME has the good efficiency demonstrated by the higher partition equilibrium constant (K{sub lh}) values and concentration factor (CF) values. The limits of detection (LOD) were 1.5-3.2 ng. The amounts of eugenol, β-caryophyllene and eugenol acetate from the clove bud sample were 1.90 mg/g, 1.47 mg/g and 7.0 mg/g, respectively. This hanging drop based method is a simple, fast and easy sample enrichment technique using minimal solvent. HSLPME is an alternative sample preparation method for the analysis of volatile aroma compounds by GC-MS.

  20. Immersed single-drop microextraction interfaced with sequential injection analysis for determination of Cr(VI) in natural waters by electrothermal-atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Pena, Francisco; Lavilla, Isela; Bendicho, Carlos

    2008-01-01

    Single-drop microextraction (SDME) and sequential injection analysis have been hyphenated for ultratrace metal determination by Electrothermal-Atomic Absorption Spectrometry (ETAAS). The novel method was targeted on extraction of the Cr(VI)-APDC chelate and encompasses the potential of SDME as a miniaturized and virtually solvent-free preconcentration technique, the ability of sequential injection analysis to handle samples and the versatility of furnace autosamplers for introducing microliter samples in ETAAS. The variables influencing the microextraction of Cr(VI) onto an organic solvent drop, i.e., type of organic solvent, microextraction time, stirring rate of the sample solution, drop volume, immersion depth of the drop, salting-out effect, temperature of the sample, concentration of the complexing agent and pH of the sample solution were fully investigated. For a 5 and 20 min microextraction time, the preconcentration factors were 20 and 70, respectively. The detection limit was 0.02 μg/L of Cr(VI) and the repeatability expressed as relative standard deviation was 7%. The SDME-SIA-ETAAS technique was validated against BCR CRM 544 (lyophilized solution) and applied to ultrasensitive determination of Cr(VI) in natural waters

  1. Miniaturized and green method for determination of chemical oxygen demand using UV-induced oxidation with hydrogen peroxide and single drop microextraction

    International Nuclear Information System (INIS)

    Akhoundzadeh, Jeyran; Chamsaz, Mahmoud; Costas, Marta; Lavilla, Isela; Bendicho, Carlos

    2013-01-01

    We report on a green method for the determination of low levels of chemical oxygen demand. It is based on the combination of (a) UV-induced oxidation with hydrogen peroxide, (b) headspace single-drop microextraction with in-drop precipitation, and (c) micro-turbidimetry. The generation of CO 2 after photolytic oxidation followed by its sequestration onto a microdrop of barium hydroxide gives rise to a precipitate of barium carbonate which is quantified by turbidimetry. UV-light induced oxidation was studied in the absence and presence of H 2 O 2 , ultrasound, and ferrous ion. Determinations of chemical oxygen demand were performed using potassium hydrogen phthalate as a model compound. The optimized method gives a calibration curve that is linear between 3.4 and 20 mg L −1 oxygen. The detection limit was 1.2 mg L −1 of oxygen, and the repeatability (as relative standard deviation) was around 5 %. The method was successfully applied to the determination of chemical oxygen demand in different natural waters and a synthetic wastewater. (author)

  2. Direct immersion single drop micro-extraction method for multi-class pesticides analysis in mango using GC-MS.

    Science.gov (United States)

    Pano-Farias, Norma S; Ceballos-Magaña, Silvia G; Muñiz-Valencia, Roberto; Jurado, Jose M; Alcázar, Ángela; Aguayo-Villarreal, Ismael A

    2017-12-15

    Due the negative effects of pesticides on environment and human health, more efficient and environmentally friendly methods are needed. In this sense, a simple, fast, free from memory effects and economical direct-immersion single drop micro-extraction (SDME) method and GC-MS for multi-class pesticides determination in mango samples was developed. Sample pre-treatment using ultrasound-assisted solvent extraction and factors affecting the SDME procedure (extractant solvent, drop volume, stirring rate, ionic strength, time, pH and temperature) were optimized using factorial experimental design. This method presented high sensitive (LOD: 0.14-169.20μgkg -1 ), acceptable precision (RSD: 0.7-19.1%), satisfactory recovery (69-119%) and high enrichment factors (20-722). Several obtained LOQs are below the MRLs established by the European Commission; therefore, the method could be applied for pesticides determination in routing analysis and custom laboratories. Moreover, this method has shown to be suitable for determination of some of the studied pesticides in lime, melon, papaya, banana, tomato, and lettuce. Copyright © 2017 Elsevier Ltd. All rights reserved.

  3. Ultrasensitive determination of mercury in human saliva by atomic fluorescence spectrometry based on solidified floating organic drop microextraction

    International Nuclear Information System (INIS)

    Yuan, C.-G.; Wang, J.; Jin, Y.

    2012-01-01

    We report on a new, rapid and simple method for the determination of ultra-trace quantities of mercury ion in human saliva. It is based on solidified floating organic drop microextraction and detection by cold vapor atomic fluorescence spectrometry (CV-AFS). Mercury ion was complexed with diethyldithiocarbamate, and the hydrophobic complex was then extracted into fine droplets of 1-undecanol. By cooling in an ice bath after extraction, the droplets in solution solidify to form a single ball floating on the surface of solution. The solidified micro drop containing the mercury complex was then transferred for determination by CV-AFS. The effects of pH value, concentration of chelating reagent, quantity of 1-undecanol, sample volume, equilibration temperature and time were investigated. Under the optimum conditions, the preconcentration of a 25-mL sample is accomplished with an enrichment factor of 182. The limit of detection is 2.5 ng L -1 . The relative standard deviation for seven replicate determinations at 0.1 ng mL -1 level is 4.1%. The method was applied to the determination of mercury in saliva samples collected from four volunteers. Two volunteers having dental amalgam fillings had 0.4 ng mL -1 mercury in their saliva, whereas mercury was not detectable in the saliva of two volunteers who had no dental fillings. (author)

  4. Sensitive analysis of amino acids with carrier-mediated single drop microextraction in-line coupled with capillary electrophoresis.

    Science.gov (United States)

    Choi, Jeongmi; Choi, Kihwan; Kim, Jihye; Ahmed, Ahmed Yacine Badjah Hadj; Al-Othman, Zeid A; Chung, Doo Soo

    2011-10-14

    In order to analyze amino acids sensitively without derivatization, we have developed carrier-mediated single drop microextraction (SDME). Nonane-1-sulfonic acid was added to an acidic sample donor solution as a carrier to form neutral ion pair complexes with amino acids. The ion pair complexes were extracted to the organic phase, covering a drop of an aqueous basic acceptor phase hanging at the tip of a capillary, and then back-extracted to the basic acceptor phase, where both the amino acids and the carrier have negative charges and the ion pair complexes are broken. The resulting extract of enriched amino acids was injected into the capillary and analyzed by capillary electrophoresis. With 20-min SDME with agitation of the donor phase, enrichment factors of four aromatic amino acids were up to 120-fold, yielding the LOD of 70-500 nM. The linear dynamic ranges for corrected peak areas were 1-100 μM with linear correlation coefficients larger than 0.9959. With internal standardization, the intraday RSDs of migration times and corrected peak areas were 0.01-0.04% and 2.0-3.7%, respectively. The capabilities of sample cleanup including desalting and preconcentration of carrier-mediated SDME were demonstrated with the analysis of human urine after minimal pretreatment of acidification and centrifugation. Copyright © 2011. Published by Elsevier B.V.

  5. A Method Based on Ultrasound-assisted Solidification of Floating Drop Microextraction Technique for the Spectrophotometric Determination of Curcumin in Turmeric Powder

    OpenAIRE

    Abbas Afkhami; Massoumeh Pirdadeh-Beiranvand; Tayyebeh Madrakian

    2017-01-01

    A method based on the ultrasound-assisted solidification of floating drop microextraction technique was developed for the spectrophotometric and spectrofluorimetric determination of curcumin in turmeric powder. In this work a small volume of an organic solvent was floated on the surface of an aqueous solution. After sonication the organic solvent is solidified and separated. The effect of extraction parameters such as type and the volume of organic solvent, temperature, salt addition and expo...

  6. Determination of patulin in apple juice by single-drop liquid-liquid-liquid microextraction coupled with liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Li, Xianjiang; Li, Hongmei; Ma, Wen; Guo, Zhen; Li, Xiaomin; Li, Xiuqin; Zhang, Qinghe

    2018-08-15

    Quick and simple analytical methodology has been developed for the measurement of patulin in apple juice by combining single-drop liquid-liquid-liquid microextraction with isotope dilution ultra-high performance liquid chromatography-mass spectrometry. After systematic parameters optimization, the whole sample pretreatment only consisted of single extraction that consumed 1.5 mL ethyl acetate. While, other methods usually needed complicated pretreatment, including extraction, purification, evaporation and redissolution. This sample pretreatment method could greatly lower the interferences from sugar-rich matrix, and the limit of detection was 0.5 μg/L and limit of quantification was 2 μg/L in apple juice. Moreover, linear range covered three orders of magnitude from 2 to 2000 μg/L. The proposed method is promising for patulin extraction and detection in apple juice, which will opens a new perspective in the enrichment of trace contaminations in high sugar complex matrix. Copyright © 2018. Published by Elsevier Ltd.

  7. Solid-Phase Extraction Followed by Dispersive Liquid-Liquid Microextraction Based on Solidification of Floating Organic Drop for the Determination of Parabens.

    Science.gov (United States)

    Hashemi, Beshare; Shamsipur, Mojtaba; Fattahi, Nazir

    2015-09-01

    A dispersive liquid-liquid microextraction based on solidification of floating organic drop method combined with solid-phase extraction (500-mg C18 sorbent) was developed for preconcentration and determination of some parabens. The experimental parameters influencing the extraction efficiency such as the type of extraction and disperser solvents, as well as their volumes, breakthrough volume, flow rate and salt addition were studied and optimized. The optimum experimental conditions found included: sample volume, 100 mL; KCl concentration, 1% (w/v); extraction solvent (1-undecanol) volume, 20 µL and disperser solvent (acetone) volume, 250 µL. Under the optimum experimental conditions, calibration graphs were linear in the range of 1-200 µg L(-1) with limits of detection ranged from 0.3 to 1.7 µg L(-1). The relative standard deviations were in the range of 1.2-3.1% (n = 5). The enrichment factors and absolute recoveries of parabens in different matrices were 245-1886 and 9.0-69.8%, respectively. The method was applied to the simultaneous determination of parabens in different matrices. The relative recoveries from water, shampoo and mouth rinse samples, which have been spiked at different levels of parabens, were 87.83-112.25%, 82.80-108.40% and 90.10-97.60%, respectively. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  8. Speciation and determination of ultra trace amounts of chromium by solidified floating organic drop microextraction (SFODME) and graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Moghadam, Masoud Rohani; Dadfarnia, Shayessteh; Haji Shabani, Ali Mohammad

    2011-01-01

    Solidified floating organic drop microextraction (SFODME) method in combination with graphite furnace atomic absorption spectrometry (GFAAS) has been used for the determination of chromium species in water and urine samples. 1-undecanol containing 2-thenoyltrifluoroacetone (TTA) was used as a selective chelating agent for the extraction of Cr(III). The total Cr was determined after the reduction of Cr(VI) to Cr(III) with hydroxylamine. The concentration of Cr(VI) was determined from the difference between the concentration of total chromium and the Cr(III). Several variables such as the sample pH, concentration of TTA, salt concentration, extraction time and the sample volume were investigated in detail. Under the optimum conditions, the limit of detection of the proposed method was 0.006 μg l -1 for Cr(III) and the relative standard deviation for six replicate determinations at 0.1 μg l -1 Cr(III) was 5.1%. The proposed method was successfully applied for the determination of chromium species in tap water, well water, mineral water, and urine samples.

  9. On-line liquid phase micro-extraction based on drop-in-plug sequential injection lab-at-valve platform for metal determination

    International Nuclear Information System (INIS)

    Mitani, Constantina; Anthemidis, Aristidis N.

    2013-01-01

    Highlights: ► Drop-in-plug micro-extraction based on SI-LAV platform for metal preconcentration. ► Automatic liquid phase micro-extraction coupled with FAAS. ► Organic solvents with density higher than water are used. ► Lead determination in environmental water and urine samples. -- Abstract: A novel automatic on-line liquid phase micro-extraction method based on drop-in-plug sequential injection lab-at-valve (LAV) platform was proposed for metal preconcentration and determination. A flow-through micro-extraction chamber mounted at the selection valve was adopted without the need of sophisticated lab-on-valve components. Coupled to flame atomic absorption spectrometry (FAAS), the potential of this lab-at-valve scheme is demonstrated for trace lead determination in environmental and biological water samples. A hydrophobic complex of lead with ammonium pyrrolidine dithiocarbamate (APDC) was formed on-line and subsequently extracted into an 80 μL plug of chloroform. The extraction procedure was performed by forming micro-droplets of aqueous phase into the plug of the extractant. All critical parameters that affect the efficiency of the system were studied and optimized. The proposed method offered good performance characteristics and high preconcentration ratios. For 10 mL sample consumption an enhancement factor of 125 was obtained. The detection limit was 1.8 μg L −1 and the precision expressed as relative standard deviation (RSD) at 50.0 μg L −1 of lead was 2.9%. The proposed method was evaluated by analyzing certified reference materials and applied for lead determination in natural waters and urine samples

  10. Liquid-phase microextraction combined with graphite furnace atomic absorption spectrometry: A review.

    Science.gov (United States)

    de la Calle, Inmaculada; Pena-Pereira, Francisco; Lavilla, Isela; Bendicho, Carlos

    2016-09-14

    An overview of the combination of liquid-phase microextraction (LPME) techniques with graphite furnace atomic absorption spectrometry (GFAAS) is reported herein. The high sensitivity of GFAAS is significantly enhanced by its association with a variety of miniaturized solvent extraction approaches. LPME-GFAAS thus represents a powerful combination for determination of metals, metalloids and organometallic compounds at (ultra)trace level. Different LPME modes used with GFAAS are briefly described, and the experimental parameters that show an impact in those microextraction processes are discussed. Special attention is paid to those parameters affecting GFAAS analysis. Main issues found when coupling LPME and GFAAS, as well as those strategies reported in the literature to solve them, are summarized. Relevant applications published on the topic so far are included. Copyright © 2016 Elsevier B.V. All rights reserved.

  11. Development of on-line single-drop micro-extraction sequential injection system for electrothermal atomic absorption spectrometric determination of trace metals

    International Nuclear Information System (INIS)

    Anthemidis, Aristidis N.; Adam, Ibrahim S.I.

    2009-01-01

    A novel automatic sequential injection (SI) single-drop micro-extraction (SDME) system is proposed as versatile approach for on-line metal preconcentration and/or separation. Coupled to electrothermal atomic absorption spectrometry (ETAAS) the potentials of this SI scheme are demonstrated for trace cadmium determination in water samples. A non-charged complex of cadmium with ammonium diethyldithiophosphate (DDPA) was produced and extracted on-line into a 60 μL micro-drop of di-isobutyl ketone (DIBK). The extraction procedure was performed into a newly designed flow-through extraction cell coupled on a sequential injection manifold. As the complex Cd(II)-DDPA flowed continuously around the micro-droplet, the analyte was extracting into the solvent micro-drop. All the critical parameters were optimized and offered good performance characteristics and high preconcentration ratios. For 600 s micro-extraction time, the enhancement factor was 10 and the sampling frequency was 6 h -1 . The detection limit was 0.01 μg L -1 and the precision (RSD at 0.1 μg L -1 of cadmium) was 3.9%. The proposed method was evaluated by analyzing certified reference material

  12. Coumarins as turn on/off fluorescent probes for detection of residual acetone in cosmetics following headspace single-drop microextraction.

    Science.gov (United States)

    Cabaleiro, N; de la Calle, I; Bendicho, C; Lavilla, I

    2014-11-01

    In this work, a new method based on headspace-single drop microextraction for the determination of residual acetone in cosmetics by microfluorospectrometry is proposed. Acetone causes fluorescence changes in a 2.5 µL-ethanolic drop (40% v/v) containing 3.10(-4) mol L(-1) 7-hydroxy-4-methylcoumarin ('turn off') or 6.10(-6) mol L(-1) 7-diethylamino-4-methylcoumarin ('turn on'). Polarity and ability to form hydrogen bonds of short chain alcohols (polar protic solvents) were crucial in order to observe these changes in the presence of acetone (polar aprotic solvent). Parameters related with the HS-SDME procedure were studied, namely headspace volume, composition, volume and temperature of drop, microextraction time, stirring rate, mass and temperature of sample, as well as the effect of potential interferents (alcohols and fragrances). The high volatility of acetone allows its extraction from an untreated cosmetic sample within 3 min. A detection limit of 0.26 µg g(-1) and repeatability, expressed as relative standard deviation, around 5% were reached. Accuracy of the proposed methodology was evaluated by means of recovery studies. The method was successfully used to analyze different cosmetics. Simplicity and high sample throughput can be highlighted. Copyright © 2014 Elsevier B.V. All rights reserved.

  13. Determination of residual 1,4-dioxane in surfactants and cleaning agents using headspace single-drop microextraction followed by gas chromatography-flame ionization detection.

    Science.gov (United States)

    Saraji, M; Shirvani, N

    2017-02-01

    Polyethoxylated surfactants are widely used in the formulation of different cleaning agents such as shampoo, dish washing and hand washing products and lotion formulation. During the production of polyethoxylated surfactants, 1,4-dioxane as a toxic and carcinogenic by-product is formed. A simple low-cost method based on headspace single-drop microextraction combined with gas chromatography-flame ionization detection was developed for the determination of 1,4-dioxane in surfactants and cleaning agents. In this method, 1,4-dioxane was extracted from 8.0 mL sample solution into a microdrop of an organic solvent, and then, it was injected to gas chromatography. The effects of such parameters as the solvent type, salt addition, microdrop volume, stirring rate, equilibrium time, extraction time and the temperature of sample solution on the extraction performance were studied and optimized. An ethoxylated surfactant containing 1,4-dioxane was used as the sample for the optimization of the extraction parameters. The linear range, determination coefficient, limit of detection and relative standard deviation of the method were 0.5-100 μg g -1 , 0.9977, 0.4 μg g -1 and 7.2% (n = 5), respectively. Different real samples including sodium lauryl ether sulphate, sodium lauryl sulphate (SLS), four brands of shampoo, and hand washing and dish washing liquids were analysed by the method. 1,4-Dioxane was detected at the concentration range of 2.4-201 μg g -1 in the samples, except dish washing liquid and SLS. A new method with the merits of simplicity, low cost, low organic solvent consumption, short analysis time, good repeatability and suitable detection limit was developed for the analysis of 1,4-dioxane in surfactants and cleaning agents. © 2016 Society of Cosmetic Scientists and the Société Française de Cosmétologie.

  14. Ultrasonic nebulization extraction-heating gas flow transfer-headspace single drop microextraction of essential oil from pericarp of Zanthoxylum bungeanum Maxim.

    Science.gov (United States)

    Wei, Shigang; Zhang, Huihui; Wang, Yeqiang; Wang, Lu; Li, Xueyuan; Wang, Yinghua; Zhang, Hanqi; Xu, Xu; Shi, Yuhua

    2011-07-22

    The ultrasonic nebulization extraction-heating gas flow transfer coupled with headspace single drop microextraction (UNE-HGFT-HS-SDME) was developed for the extraction of essential oil from Zanthoxylum bungeanum Maxim. The gas chromatography-mass spectrometry was applied to the determination of the constituents in the essential oil. The contents of the constituents from essential oil obtained by the proposed method were found to be more similar to those obtained by hydro-distillation (HD) than those obtained by ultrasonic nebulization extraction coupled with headspace single drop microextraction (UNE-HS-SDME). The heating gas flow was firstly used in the analysis of the essential oil to transfer the analytes from the headspace to the solvent microdrop. The relative standard deviations for determining the five major constituents were in the range from 1.5 to 6.7%. The proposed method is a fast, sensitive, low cost and small sample consumption method for the determination of the volatile and semivolatile constituents in the plant materials. Copyright © 2011 Elsevier B.V. All rights reserved.

  15. Collective Ion-Pair Single-Drop Microextraction Attenuated Total Reflectance Fourier Transform Infrared Spectroscopic Determination of Perchlorate in Bioenvironmental Samples.

    Science.gov (United States)

    Chandrawanshi, Swati; Verma, Santosh K; Deb, Manas K

    2017-09-28

    Perchlorate (ClO₄ - ) is an environmental pollutant that affects human health. Perchlorate acts as a competitive inhibitor of iodine uptake in the thyroid gland (sodium-iodide symporter inhibitor); thus, its determination is important for public health concerns. Water and milk constitute a significant portion of the human diet. Because regular intake leads to an increase in perchlorate concentration in the human body, the estimation of perchlorate is of great concern. In this work, ion-pair single-drop microextraction (SDME) combined with attenuated total reflectance (ATR)-FTIR spectroscopy has been developed for the determination of perchlorate in bioenvironmental (soil, water, dairy milk, breast milk, and urine) samples. Perchlorate was extracted in a single drop of methyl isobutyl ketone as an - with the cationic surfactant cetyltrimethylammonuim bromide under optimized conditions. The strongest IR peak (at 1076 cm -1 ) was selected for the quantification of perchlorate among three observed vibrational peaks. Eight calibration curves for different concentration ranges of perchlorate were prepared, and excellent linearity was observed for absorbance and peak area in the range of 0.03-100 ng/mL perchlorate, with r values of 0.977 and 0.976, respectively. The RSDs ( n = 8) for the perchlorate concentration ranges of 0.03-100, 0.03-0.5, 0.5-10, and 10-100 ng/mL were in the range of 1.9-2.7% for the above calibration curves. The LOD and LOQ in the present work were 0.003 and 0.02 ng/mL, respectively. The extracted microdrop was analyzed directly by ATR-FTIR spectroscopy. The parameters affecting SDME, i.e, effect of pH, stirring rate, reagent concentration, microdrop volume, and extraction time, were optimized, and the role of foreign species was also investigated. F - and t -tests were performed to check the analytical QA of the method. A noteworthy feature of the reported method is the noninterference of any of the associated ions. The results were compared with

  16. Determining heterocyclic aromatic amines in aqueous samples: A novel dispersive liquid-liquid micro-extraction method based on solidification of floating organic drop and ultrasound assisted back extraction followed by UPLC-MS/MS.

    Science.gov (United States)

    Canales, Romina; Guiñez, María; Bazán, Cristian; Reta, Mario; Cerutti, Soledad

    2017-11-01

    A novel dispersive liquid-liquid microextraction based on solidification of floating organic droplet combined with ultrasound assisted back extraction for the determination of four heterocyclic aromatic amines in natural water samples prior ultra high-performance liquid chromatography-tandem mass spectrometry was developed. The analytes were extracted from the water samples by a dispersive liquid-liquid microextraction procedure based on solidification of floating organic drop, which was performed by a mixture composed by a less dense than water extraction solvent, 1-undecanol, and a dispersive solvent, methanol. After that, a novel ultrasound assisted back extraction step was performed in order to make the clean-up/enrichment procedure compatible with the detection requirements. Under optimum conditions, linearity ranged from 2.2 to 50ngmL -1 , with enrichment factors from 130 to 136-folds. Thus limits of detection between 0.7 and 2.9ngmL -1 were obtained. Precision of the method was evaluated in terms of repeatability, relative standard deviations varied from 4.3% to 6.7%. Relative recoveries ranged from 92% to 106% for all analytes. The satisfactory performance demonstrated that the proposed methodology has a strong potential for application in the multi-residue analysis of heterocyclic aromatic amines present in complex environmental matrices. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. Reversed-phase single drop microextraction followed by high-performance liquid chromatography with fluorescence detection for the quantification of synthetic phenolic antioxidants in edible oil samples.

    Science.gov (United States)

    Farajmand, Bahman; Esteki, Mahnaz; Koohpour, Elham; Salmani, Vahid

    2017-04-01

    The reversed-phase mode of single drop microextraction has been used as a preparation method for the extraction of some phenolic antioxidants from edible oil samples. Butylated hydroxyl anisole, tert-butylhydroquinone and butylated hydroxytoluene were employed as target compounds for this study. High-performance liquid chromatography followed by fluorescence detection was applied for final determination of target compounds. The most interesting feature of this study is the application of a disposable insulin syringe with some modification for microextraction procedure that efficiently improved the volume and stability of the solvent microdrop. Different parameters such as the type and volume of solvent, sample stirring rate, extraction temperature, and time were investigated and optimized. Analytical performances of the method were evaluated under optimized conditions. Under the optimal conditions, relative standard deviations were between 4.4 and 10.2%. Linear dynamic ranges were 20-10 000 to 2-1000 μg/g (depending on the analytes). Detection limits were 5-670 ng/g. Finally, the proposed method was successfully used for quantification of the antioxidants in some edible oil samples prepared from market. Relative recoveries were achieved from 88 to 111%. The proposed method had a simplicity of operation, low cost, and successful application for real samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Solidified Floating Organic Drop Microextraction for the Detection of Trace Amount of Lead in Various Samples by Electrothermal Atomic Absorption Spectrometry

    Directory of Open Access Journals (Sweden)

    Oya Aydın Urucu

    2017-01-01

    Full Text Available A novel method was developed for determination of trace amounts of lead in water and food samples. Solidified floating organic drop microextraction was used to preconcentrate the lead ion. After the analyte was complexed with 1-(2-pyridylazo-2-naphthol, undecanol and acetonitrile were added as extraction and dispersive solvent, respectively. Variables such as pH, volumes of extraction and dispersive solvents, and concentration of chelating agent were optimized. Under the optimum conditions, the detection limit of Pb (II was determined as 0.042 µg L−1 with an enrichment factor of 300. The relative standard deviation is <10%. Accuracy of the developed procedure was evaluated by the analysis of certified reference material of human hair (NCS DC 73347 and wastewater (SPS-WW2 with satisfactory results. The developed procedure was then successfully applied to biscuit and water samples for detection of Pb (II ions.

  19. Ultra-Trace Determination of Copper and Silver in Environmental Samples by Using Ionic Liquid-Based Single Drop Microextraction-Electrothermal Atomic Absorption Spectrometry

    Directory of Open Access Journals (Sweden)

    J. Abolhasani

    2013-11-01

    Full Text Available A sensitive, selective and effective ionic liquid-based single drop microextraction technique wasdeveloped by using ionic liquid, 1-hexyl-3-methylimidazolium hexafluorophosphate, C6MIMPF6, coupledwith electrothermal atomic absorption spectrometry (ETAAS for the determination of copper and silver inenvironmental samples. Dithizone was used as chelating agent. Several factors that influence themicroextraction efficiency and ETAAS signal, such as pH, dithizone concentration, extraction time, amounts ofionic liquid, stirring rate, pyrolysis and atomization temperature were investigated and the microextractionconditions were established. In the optimum experimental conditions, the detection limits (3 s of the methodwere 4 and 8 ng L-1 and corresponding relative standard deviations (0.1 μg L-1, n = 6 were 4.2% and 4.8% forAg and Cu, respectively. The developed method was validated by analysis of a certified reference material andapplied to the determination of silver and copper.

  20. Direct solid-phase microextraction combined with gas and liquid chromatography for the determination of lidocaine in human urine

    NARCIS (Netherlands)

    Koster, E.H M; Hofman, N.S K; de Jong, G.J.

    Solid-phase microextraction (SPME) has been combined with gas chromatography (GC) and liquid chromatography (LC) for the determination of lidocaine in human urine. A polydimethylsiloxane (PDMS) coated fibre was directly immersed into buffered urine. Extraction conditions such as time, pH, ionic

  1. A novel solidified floating organic drop microextraction method for preconcentration and determination of copper ions by flow injection flame atomic absorption spectrometry.

    Science.gov (United States)

    Sahin, Ciğdem Arpa; Tokgöz, Ilknur

    2010-05-14

    A rapid, simple and cost effective solidified floating organic drop microextraction (SFODME) and flow injection flame atomic absorption spectrometric determination (FI-FAAS) method for copper was developed. In this method, a free microdrop of 1-undecanol containing 1,5-diphenyl carbazide (DPC) as the complexing agent was transferred to the surface of an aqueous sample including Cu(II) ions, while being agitated by a stirring bar in the bulk of the solution. Under the proper stirring conditions, the suspended microdrop can remain at the top-center position of the aqueous sample. After the completion of the extraction, the sample vial was cooled by placing it in a refrigerator for 10min. The solidified microdrop was then transferred into a conical vial, where it melted immediately and diluted to 300microL with ethanol. Finally, copper ions in 200microL of diluted solution were determined by FI-FAAS. Several factors affecting the microextraction efficiency, such as type of extraction solvent, pH, complexing agent concentration, extraction time, stirring rate, sample volume and temperature were investigated and optimized. Under optimized conditions for 100mL of solution, the preconcentration factor was 333 and the enrichment factor was 324. The limit of detection (3s) was 0.4ngmL(-1), the limit of quantification (10s) was 1.1ngmL(-1) and the relative standard deviation (RSD) for 10 replicate measurements of 10ngmL(-1) copper was 0.9%. The proposed method was successfully applied to the determination of copper in different water samples. Copyright 2010 Elsevier B.V. All rights reserved.

  2. Rapid analysis of Fructus forsythiae essential oil by ionic liquids-assisted microwave distillation coupled with headspace single-drop microextraction followed by gas chromatography–mass spectrometry

    International Nuclear Information System (INIS)

    Jiao, Jiao; Ma, Dan-Hui; Gai, Qing-Yan; Wang, Wei; Luo, Meng; Fu, Yu-Jie; Ma, Wei

    2013-01-01

    Graphical abstract: -- Highlights: •A new ILAMD-HS-SDME method is developed for the microextraction of essential oil. •ILs used as destruction agent of plant cell walls and microwave absorption medium. •Parameters affecting the extraction efficiency are optimized by Box–Behnken design. •Procedure benefits: similar constituents, shorter duration and smaller sample amount. •ILAMD-HS-SDME followed by GC–MS is a promising technique in analytical fields. -- Abstract: A rapid, green and effective miniaturized sample preparation and analytical technique, i.e. ionic liquids-assisted microwave distillation coupled with headspace single-drop microextraction (ILAMD-HS-SDME) followed by gas chromatography–mass spectrometry (GC–MS) was developed for the analysis of essential oil (EO) in Fructus forsythiae. In this work, ionic liquids (ILs) were not only used as the absorption medium of microwave irradiation but also as the destruction agent of plant cell walls. 1-Ethyl-3-methylimidazolium acetate ([C 2 mim]OAc) was chosen as the optimal ILs. Moreover, n-heptadecane (2.0 μL) was selected as the appropriate suspended solvent for the extraction and concentration of EO. Extraction conditions of the proposed method were optimized using the relative peak area of EO constituents as the index, and the optimal operational parameters were obtained as follows: irradiation power (300 W), sample mass (0.7 g), mass ratio of ILs to sample (2.4), temperature (78 °C) and time (3.4 min). In comparison to previous reports, the proposed method was faster and required smaller sample amount but could equally monitor all EO constituents with no significant differences

  3. A novel solidified floating organic drop microextraction method for preconcentration and determination of copper ions by flow injection flame atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Sahin, Cigdem Arpa; Tokgoez, Ilknur

    2010-01-01

    A rapid, simple and cost effective solidified floating organic drop microextraction (SFODME) and flow injection flame atomic absorption spectrometric determination (FI-FAAS) method for copper was developed. In this method, a free microdrop of 1-undecanol containing 1,5-diphenyl carbazide (DPC) as the complexing agent was transferred to the surface of an aqueous sample including Cu(II) ions, while being agitated by a stirring bar in the bulk of the solution. Under the proper stirring conditions, the suspended microdrop can remain at the top-center position of the aqueous sample. After the completion of the extraction, the sample vial was cooled by placing it in a refrigerator for 10 min. The solidified microdrop was then transferred into a conical vial, where it melted immediately and diluted to 300 μL with ethanol. Finally, copper ions in 200 μL of diluted solution were determined by FI-FAAS. Several factors affecting the microextraction efficiency, such as type of extraction solvent, pH, complexing agent concentration, extraction time, stirring rate, sample volume and temperature were investigated and optimized. Under optimized conditions for 100 mL of solution, the preconcentration factor was 333 and the enrichment factor was 324. The limit of detection (3 s) was 0.4 ng mL -1 , the limit of quantification (10 s) was 1.1 ng mL -1 and the relative standard deviation (RSD) for 10 replicate measurements of 10 ng mL -1 copper was 0.9%. The proposed method was successfully applied to the determination of copper in different water samples.

  4. Rapid analysis of Fructus forsythiae essential oil by ionic liquids-assisted microwave distillation coupled with headspace single-drop microextraction followed by gas chromatography–mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Jiao, Jiao [State Key Laboratory of Tree Genetics and Breeding, Northeast Forestry University, Harbin 150040 (China); Ma, Dan-Hui [College of Life Sciences, Northeast Forestry University, Harbin 150040 (China); Gai, Qing-Yan; Wang, Wei; Luo, Meng [State Engineering Laboratory of Bio-Resource Eco-Utilization, Northeast Forestry University, Harbin 150040 (China); Fu, Yu-Jie, E-mail: yujie_fu2002@yahoo.com [State Engineering Laboratory of Bio-Resource Eco-Utilization, Northeast Forestry University, Harbin 150040 (China); Ma, Wei, E-mail: mawei@hljucm.net [State Key Laboratory of Tree Genetics and Breeding, Northeast Forestry University, Harbin 150040 (China); School of Pharmaceutical, Heilongjiang University of Chinese Medicine, Harbin 150040 (China)

    2013-12-04

    Graphical abstract: -- Highlights: •A new ILAMD-HS-SDME method is developed for the microextraction of essential oil. •ILs used as destruction agent of plant cell walls and microwave absorption medium. •Parameters affecting the extraction efficiency are optimized by Box–Behnken design. •Procedure benefits: similar constituents, shorter duration and smaller sample amount. •ILAMD-HS-SDME followed by GC–MS is a promising technique in analytical fields. -- Abstract: A rapid, green and effective miniaturized sample preparation and analytical technique, i.e. ionic liquids-assisted microwave distillation coupled with headspace single-drop microextraction (ILAMD-HS-SDME) followed by gas chromatography–mass spectrometry (GC–MS) was developed for the analysis of essential oil (EO) in Fructus forsythiae. In this work, ionic liquids (ILs) were not only used as the absorption medium of microwave irradiation but also as the destruction agent of plant cell walls. 1-Ethyl-3-methylimidazolium acetate ([C{sub 2}mim]OAc) was chosen as the optimal ILs. Moreover, n-heptadecane (2.0 μL) was selected as the appropriate suspended solvent for the extraction and concentration of EO. Extraction conditions of the proposed method were optimized using the relative peak area of EO constituents as the index, and the optimal operational parameters were obtained as follows: irradiation power (300 W), sample mass (0.7 g), mass ratio of ILs to sample (2.4), temperature (78 °C) and time (3.4 min). In comparison to previous reports, the proposed method was faster and required smaller sample amount but could equally monitor all EO constituents with no significant differences.

  5. Determination of methylmercury by electrothermal atomic absorption spectrometry using headspace single-drop microextraction with in situ hydride generation

    International Nuclear Information System (INIS)

    Gil, Sandra; Fragueiro, Sandra; Lavilla, Isela; Bendicho, Carlos

    2005-01-01

    A new method is proposed for preconcentration and matrix separation of methylmercury prior to its determination by electrothermal atomic absorption spectrometry (ETAAS). Generation of methylmercury hydride (MeHgH) from a 5-ml solution is carried out in a closed vial and trapped onto an aqueous single drop (3-μl volume) containing Pd(II) or Pt(IV) (50 and 10 mg/l, respectively). The hydrogen evolved in the headspace (HS) after decomposition of sodium tetrahydroborate (III) injected for hydride generation caused the formation of finely dispersed Pd(0) or Pt(0) in the drop, which in turn, were responsible for the sequestration of MeHgH. A preconcentration factor of ca. 40 is achieved with both noble metals used as trapping agents. The limit of detection of methylmercury was 5 and 4 ng/ml (as Hg) with Pd(II) or Pt(IV) as trapping agents, and the precision expressed as relative standard deviation was about 7%. The preconcentration system was fully characterised through optimisation of the following variables: Pd(II) or Pt(IV) concentration in the drop, extraction time, pH of the medium, temperatures of both sample solution and drop, concentration of salt in the sample solution, sodium tetrahydroborate (III) concentration in the drop and stirring rate. The method has been successfully validated against two fish certified reference materials (CRM 464 tuna fish and CRM DORM-2 dogfish muscle) following selective extraction of methylmercury in 2 mol/l HCl medium

  6. Dispersive liquid-liquid microextraction based on solidification of floating organic drop for preconcentration and determination of trace amounts of copper by flame atomic absorption spectrometry.

    Science.gov (United States)

    Karadaş, Cennet; Kara, Derya

    2017-04-01

    A novel, simple, rapid, sensitive, inexpensive and environmentally friendly dispersive liquid-liquid microextraction method based on the solidification of a floating organic drop (DLLME-SFO) was developed for the determination of copper by flame atomic absorption spectrometry (FAAS). N-o-Vanillidine-2-amino-p-cresol was used as a chelating ligand and 1-undecanol was selected as an extraction solvent. The main parameters affecting the performance of DLLME-SFO, such as sample pH, volume of extraction solvent, extraction time, concentration of the chelating ligand, salt effect, centrifugation time and sample volume were investigated and optimized. The effect of interfering ions on the recovery of copper was also examined. Under the optimum conditions, the detection limit (3σ) was 0.93μgL -1 for Cu using a sample volume of 20mL, yielding a preconcentration factor of 20. The proposed method was successfully applied to the determination of Cu in tap, river and seawater, rice flour and black tea samples as well as certified reference materials. Copyright © 2016. Published by Elsevier Ltd.

  7. A selective and sensitive optical sensor for dissolved ammonia detection via agglomeration of fluorescent Ag nanoclusters and temperature gradient headspace single drop microextraction.

    Science.gov (United States)

    Dong, Jiang Xue; Gao, Zhong Feng; Zhang, Ying; Li, Bang Lin; Li, Nian Bing; Luo, Hong Qun

    2017-05-15

    In this paper, a simple sensor platform is presented for highly selective and sensitive detection of dissolved ammonia in aqueous solutions without pretreatment based on temperature gradient headspace single drop microextraction (HS-SDME) technique, and fluorescence and UV-vis spectrophotometry are utilized with the Ag nanoclusters (Ag NCs) functioned by citrate and glutathione as the probe. The sensing mechanism is based on the volatility of ammonia gas and the active response of Ag NCs to pH change caused by the introduction of ammonia. High pH can make the Ag NCs agglomerate and lead to the obvious decrease of fluorescence intensity and absorbance of Ag NCs solution. Moreover, the presented method exhibits a remarkably high selectivity toward dissolved ammonia over most of inorganic ions and amino acid, and shows a good linear range of 10-350μM (0.14-4.9mgNL -1 ) with a low detection limit of 336nM (4.70μgNL -1 ) at a signal-to-noise ratio of 3. In addition, the practical applications of the sensor have been successfully demonstrated by detecting dissolved ammonia in real samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  8. A Method Based on Ultrasound-assisted Solidification of Floating Drop Microextraction Technique for the Spectrophotometric Determination of Curcumin in Turmeric Powder

    Directory of Open Access Journals (Sweden)

    Abbas Afkhami

    2017-06-01

    Full Text Available A method based on the ultrasound-assisted solidification of floating drop microextraction technique was developed for the spectrophotometric and spectrofluorimetric determination of curcumin in turmeric powder. In this work a small volume of an organic solvent was floated on the surface of an aqueous solution. After sonication the organic solvent is solidified and separated. The effect of extraction parameters such as type and the volume of organic solvent, temperature, salt addition and exposure time, on the extraction recovery was investigated and optimized. Finally, the method droplet was used for the determination of analyte. Under the optimum extraction conditions, a linear range of 0.006–30 μg mL-1 and a relative standard deviation (RSD of 2.72% for curcumin wasachieved. Limits of detection of 7 and 2 ng mL-1 curcumin was obtained for the spectrophotometric and spectrofluometric methods, respectively. The obtained results show that the application of this method can be successful for the analysis of curcumin in turmeric powder samples.

  9. Ultrasound-assisted single-drop microextraction for the determination of cadmium in vegetable oils using high-resolution continuum source electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Almeida, Jorge S.; Anunciação, Taiana A. [Departamento de Química Analítica, Instituto de Química, Universidade Federal da Bahia, Campus Universitário de Ondina, Salvador, Bahia 40170-280 (Brazil); Brandão, Geovani C. [Departamento de Química Analítica, Instituto de Química, Universidade Federal da Bahia, Campus Universitário de Ondina, Salvador, Bahia 40170-280 (Brazil); INCT de Energia e Ambiente, Instituto de Química, Universidade Federal da Bahia, Campus Universitário de Ondina, Salvador, Bahia 40170-280 (Brazil); Dantas, Alailson F. [Departamento de Química Analítica, Instituto de Química, Universidade Federal da Bahia, Campus Universitário de Ondina, Salvador, Bahia 40170-280 (Brazil); Lemos, Valfredo A. [Laboratório de Química Analítica (LQA), Universidade Estadual do Sudoeste da Bahia, Campus de Jequié, Jequié, Bahia 45506-191 (Brazil); and others

    2015-05-01

    This work presents an ultrasound-assisted single-drop microextraction procedure for the determination of cadmium in vegetable oils using high-resolution continuum source electrothermal atomic absorption spectrometry. Some initial tests showed that the best extraction efficiency was obtained when using ultrasound instead of mechanical agitation, indicating that acoustic cavitation improved the extraction process. Nitric, hydrochloric and acetic acids were evaluated for use in the extraction process, and HNO{sub 3} gave the best results. A two-level full-factorial design was applied to investigate the best conditions for the extraction of Cd from the oil samples. The influences of the sonication amplitude, time and temperature of the extraction were evaluated. The results of the design revealed that all of the variables had a significant effect on the experimental results. Afterward, a Box–Behnken design was applied to determine the optimum conditions for the determination of cadmium in vegetable oil samples. According to a multivariate study, the optimum conditions were as follows: sonication amplitude of 60%, extraction time of 15 min, extraction temperature of 46 °C and 0.1 mol L{sup −1} HNO{sub 3} as the extractor solution. Under optimized conditions, the developed method allows for the determination of Cd in oil samples with a limit of quantification of 7.0 ng kg{sup −1}. Addition and recovery experiments were performed in vegetable oil samples to evaluate the accuracy of the method, and the recoveries obtained varied from 90% to 115%. The samples were also analyzed after the acid digestion procedure, and the paired t-test (95% confidence level) did not show significant differences from the proposed method. - Highlights: • The determination of cadmium in vegetable oils was developed using UA-SDME. • HR-CS ET-AAS was employed as a detection technique with direct drop sampling. • The procedure allowed for a reduction in the consumption of reagents and

  10. Rapid analysis of the essential oil components of dried Zanthoxylum bungeanum Maxim by Fe2O3-magnetic-microsphere-assisted microwave distillation and simultaneous headspace single-drop microextraction followed by GC-MS.

    Science.gov (United States)

    Ye, Qing

    2013-06-01

    In this work, microwave distillation assisted by Fe2 O3 magnetic microspheres (FMMS) and headspace single-drop microextraction were combined, and developed for determination of essential oil compounds in dried Zanthoxylum bungeanum Maxim (ZBM). The FMMS were used as microwave absorption solid medium for dry distillation of dried ZBM. Using the proposed method, isolation, extraction, and concentration of essential oil compounds can be carried out in a single step. The experimental parameters including extraction solvent, solvent volume, microwave power, irradiation time, and the amount of added FMMS, were studied. The optimal analytical conditions were: 2.0 μL decane as the extraction solvent, microwave power of 300 W, irradiation time of 2 min, and the addition of 0.1 g FMMS to ZBM. The method precision was from 4 to 10%. A total of 52 compounds were identified by the proposed method. The conventional steam distillation method was also used for the analysis of essential oil in dried ZBM and only 31 compounds were identified by steam distillation method. It was found that the proposed method is a simple, rapid, reliable, and solvent-free technique for the determination of volatile compounds in Chinese herbs. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Trace analysis of three antihistamines in human urine by on-line single drop liquid-liquid-liquid microextraction coupled to sweeping micellar electrokinetic chromatography and its application to pharmacokinetic study.

    Science.gov (United States)

    Gao, Wenhua; Chen, Yunsheng; Chen, Gaopan; Xi, Jing; Chen, Yaowen; Yang, Jianying; Xu, Ning

    2012-09-01

    A rapid and efficient dual preconcentration method of on-line single drop liquid-liquid-liquid microextraction (SD-LLLME) coupled to sweeping micellar electrokinetic chromatography (MEKC) was developed for trace analysis of three antihistamines (mizolastine, chlorpheniramine and pheniramine) in human urine. Three analytes were firstly extracted from donor phase (4 mL urine sample) adjusted to alkaline condition (0.5 M NaOH). The unionized analytes were subsequently extracted into a drop of n-octanol layered over the urine sample, and then into a microdrop of acceptor phase (100 mM H(3)PO(4)) suspended from a capillary inlet. The enriched acceptor phase was on-line injected into capillary with a height difference and then analyzed directly by sweeping MEKC. Good linear relationships were obtained for all analytes in a range of 6.25 × 10(-6) to 2.5 × 10(-4)g/L with correlation coefficients (r) higher than 0.987. The proposed method achieved limits of detections (LOD) varied from 1.2 × 10(-7) to 9.5 × 10(-7)g/L based on a signal-to-noise of 3 (S/N=3) with 751- to 1372-fold increases in detection sensitivity for analytes, and it was successfully applied to the pharmacokinetic study of three antihistamines in human urine after an oral administration. The results demonstrated that this method was a promising combination for the rapid trace analysis of antihistamines in human urine with the advantages of operation simplicity, high enrichment factor and little solvent consumption. Copyright © 2012 Elsevier B.V. All rights reserved.

  12. Combination of counter current salting-out homogenous liquid-liquid extraction and dispersive liquid-liquid microextraction as a novel microextraction of drugs in urine samples.

    Science.gov (United States)

    Akramipour, Reza; Fattahi, Nazir; Pirsaheb, Meghdad; Gheini, Simin

    2016-02-15

    The counter current salting-out homogenous liquid-liquid extraction (CCSHLLE) joined with the dispersive liquid-liquid microextraction based on solidification of floating organic drop (DLLME-SFO) has been developed as a high preconcentration technique for the determination of different drugs in urine samples. Amphetamines were employed as model compounds to assess the extraction procedure and were determined by high performance liquid chromatography-ultraviolet detection (HPLC-UV). In this method, initially, NaCl as a separation reagent is filled into a small column and a mixture of urine and acetonitrile is passed through the column. By passing the mixture, NaCl is dissolved and the fine droplets of acetonitrile are formed due to salting-out effect. The produced droplets go up through the remained mixture and collect as a separated layer. Then, the collected acetonitrile is removed with a syringe and mixed with 30.0μL 1-undecanol (extraction solvent). In the second step, the 5.00mLK2CO3 solution (2% w/v) is rapidly injected into the above mixture placed in a test tube for further DLLME-SFO. Under the optimum conditions, calibration curves are linear in the range of 1-3000μgL(-1) and limit of detections (LODs) are in the range of 0.5-2μgL(-1). The extraction recoveries and enrichment factors ranged from 78 to 84% and 157 to 168, respectively. Repeatability (intra-day) and reproducibility (inter-day) of method based on seven replicate measurements of 100μgL(-1) of amphetamines were in the range of 3.5-4.5% and 4-5%, respectively. The method was successfully applied for the determination of amphetamines in the actual urine samples. The relative recoveries of urine samples spiked with amphetamine and methamphetamine are 90-108%. Copyright © 2016 Elsevier B.V. All rights reserved.

  13. Ultrasound-assisted single-drop microextraction for the determination of cadmium in vegetable oils using high-resolution continuum source electrothermal atomic absorption spectrometry

    Science.gov (United States)

    Almeida, Jorge S.; Anunciação, Taiana A.; Brandão, Geovani C.; Dantas, Alailson F.; Lemos, Valfredo A.; Teixeira, Leonardo S. G.

    2015-05-01

    This work presents an ultrasound-assisted single-drop microextraction procedure for the determination of cadmium in vegetable oils using high-resolution continuum source electrothermal atomic absorption spectrometry. Some initial tests showed that the best extraction efficiency was obtained when using ultrasound instead of mechanical agitation, indicating that acoustic cavitation improved the extraction process. Nitric, hydrochloric and acetic acids were evaluated for use in the extraction process, and HNO3 gave the best results. A two-level full-factorial design was applied to investigate the best conditions for the extraction of Cd from the oil samples. The influences of the sonication amplitude, time and temperature of the extraction were evaluated. The results of the design revealed that all of the variables had a significant effect on the experimental results. Afterward, a Box-Behnken design was applied to determine the optimum conditions for the determination of cadmium in vegetable oil samples. According to a multivariate study, the optimum conditions were as follows: sonication amplitude of 60%, extraction time of 15 min, extraction temperature of 46 °C and 0.1 mol L- 1 HNO3 as the extractor solution. Under optimized conditions, the developed method allows for the determination of Cd in oil samples with a limit of quantification of 7.0 ng kg- 1. Addition and recovery experiments were performed in vegetable oil samples to evaluate the accuracy of the method, and the recoveries obtained varied from 90% to 115%. The samples were also analyzed after the acid digestion procedure, and the paired t-test (95% confidence level) did not show significant differences from the proposed method.

  14. Determination of lidocaine in plasma by direct solid-phase microextraction combined with gas chromatography

    NARCIS (Netherlands)

    Koster, EHM; Wemes, C; Morsink, JB; de Jong, GJ

    2000-01-01

    Direct-immersion solid-phase microextraction (SPME) has been used to extract the local anesthetic lidocaine from human plasma. A simplified model shows the relationship between the total amount of drug in plasma and the amount of drug extracted. The model takes into account that the drug

  15. Single drop based-liquid phase microextraction using ionic liquid as extractor solvent for extraction and preconcentration of copper and silver from food and water samples prior to determination by electrothermal atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    j Abolhasani

    2013-08-01

    Full Text Available A new single drop micro-extraction method based on ionic liquids was developed for the pre-concentration of ultra-traces of silver and copper prior to its determination by electro-thermal atomic absorption spectrometry (ETAAS. An 8-μL drop of ionic liquid, 1-hexyl-3-methylimidazolium hexafluorophosphate, [C6MIM][PF6], was used for the extraction of silver and copper ions as dithizone complex. Important variables affecting microextraction efficiency and ETAAS signal, such as pyrolysis and atomization temperature, dithizone concentration, extraction time, drop volume and stirring rate were investigated and optimized. Under the optimum experimental conditions, the detection limits (3 s of the method were 4 and 8 ng L-1, for Ag and Cu, respectively and corresponding relative standard deviations (0.1 μg L-1, n = 6 were 4.2% and 4.8%. The developed method was successfully applied to the determination of copper and silver in food and water samples.

  16. Fully automated ionic liquid-based headspace single drop microextraction coupled to GC-MS/MS to determine musk fragrances in environmental water samples.

    Science.gov (United States)

    Vallecillos, Laura; Pocurull, Eva; Borrull, Francesc

    2012-09-15

    A fully automated ionic liquid-based headspace single drop microextraction (IL-HS-SDME) procedure has been developed for the first time to preconcentrate trace amounts of ten musk fragrances extensively used in personal care products (six polycyclic musks, three nitro musks and one polycyclic musk degradation product) from wastewater samples prior to analysis by gas chromatography and ion trap tandem mass spectrometry (GC-IT-MS/MS). Due to the low volatility of the ILs, a large internal diameter liner (3.4 mm i.d.) was used to improve the ILs evaporation. Furthermore, a piece of glass wool was introduced into the liner to avoid the entrance of the ILs in the GC column and a guard column was used to prevent analytical column damages. The main factors influencing the IL-HS-SDME were optimized. For all species, the highest enrichments factors were achieved using 1 μL of 1-octyl-3-methylimidazolium hexafluorophosphate ([OMIM][PF(6)]) ionic liquid exposed in the headspace of 10 mL water samples containing 300 g L(-1) of NaCl and stirred at 750 rpm and 60 °C for 45 min. All compounds were determined by direct injection GC-IT-MS/MS with a chromatographic time of 19 min. Method detection limits were found in the low ng mL(-1) range between 0.010 ng mL(-1) and 0.030 ng mL(-1) depending on the target analytes. Also, under optimized conditions, the method gave good levels of intra-day and inter-day repeatabilities in wastewater samples with relative standard deviations varying between 3% and 6% and 5% and 11%, respectively (n=3, 1 ng mL(-1)). The applicability of the method was tested with different wastewater samples from influent and effluent urban wastewater treatment plants (WWTPs) and one potable treatment plant (PTP). The analysis of influent urban wastewater revealed the presence of galaxolide and tonalide at concentrations of between 2.10 ng mL(-1) and 0.29 ng mL(-1) and 0.32 ng mL(-1) and MQL (Method Quantification Limit), respectively; while the remaining

  17. Liquid-phase microextraction combined with hollow fiber as a sample preparation technique prior to gas chromatography/mass spectrometry.

    Science.gov (United States)

    Zhao, Limian; Lee, Hian Kee

    2002-06-01

    Two modes of liquid-phase microextraction (LPME) combined with hollow fiber (HF) were developed for gas chromatography/mass spectrometry (GC/MS). Both methodologies, that is, static LPME with HF and dynamic LPME with HF, involved the use of a small volume of organic solvent impregnated in the hollow fiber, which was held by the needle of a conventional GC syringe. In static LPME/HF, the hollow fiber impregnated with solvent was immersed in the aqueous sample, and the extraction processed under stirring; in dynamic LPME/HF, the solvent was repeatedly withdrawn into and discharged from the hollow fiber by a syringe pump. This is believed to be the first reported instance of a semiautomated liquid microextraction procedure. The performance of the two techniques was demonstrated in the analysis of two PAH compounds in an aqueous sample. Static LPME/HF provided approximately 35-fold enrichment in 10 min and good reproducibility (approximately 4%). Dynamic LPME/HF could provide higher enrichment (approximately 75-fold) in 10 min and even better reproducibility (approximately 3%). Both methods allow the direct transfer of extracted analytes to a GC/MS system for analysis.

  18. Determining octanol-water partition coefficients for extremely hydrophobic chemicals by combining "slow stirring" and solid-phase microextraction.

    Science.gov (United States)

    Jonker, Michiel T O

    2016-06-01

    Octanol-water partition coefficients (KOW ) are widely used in fate and effects modeling of chemicals. Still, high-quality experimental KOW data are scarce, in particular for very hydrophobic chemicals. This hampers reliable assessments of several fate and effect parameters and the development and validation of new models. One reason for the limited availability of experimental values may relate to the challenging nature of KOW measurements. In the present study, KOW values for 13 polycyclic aromatic hydrocarbons were determined with the gold standard "slow-stirring" method (log KOW 4.6-7.2). These values were then used as reference data for the development of an alternative method for measuring KOW . This approach combined slow stirring and equilibrium sampling of the extremely low aqueous concentrations with polydimethylsiloxane-coated solid-phase microextraction fibers, applying experimentally determined fiber-water partition coefficients. It resulted in KOW values matching the slow-stirring data very well. Therefore, the method was subsequently applied to a series of 17 moderately to extremely hydrophobic petrochemical compounds. The obtained KOW values spanned almost 6 orders of magnitude, with the highest value measuring 10(10.6) . The present study demonstrates that the hydrophobicity domain within which experimental KOW measurements are possible can be extended with the help of solid-phase microextraction and that experimentally determined KOW values can exceed the proposed upper limit of 10(9) . Environ Toxicol Chem 2016;35:1371-1377. © 2015 SETAC. © 2015 SETAC.

  19. Combining spray nozzle simulators with meshes: characterization of rainfall intensity and drop properties

    Science.gov (United States)

    Carvalho, Sílvia C. P.; de Lima, João L. M. P.; de Lima, M. Isabel P.

    2013-04-01

    Rainfall simulators can be a powerful tool to increase our understanding of hydrological and geomorphological processes. Nevertheless, rainfall simulators' design and operation might be rather demanding, for achieving specific rainfall intensity distributions and drop characteristics. The pressurized simulators have some advantages over the non-pressurized simulators: drops do not rely on gravity to reach terminal velocity, but are sprayed out under pressure; pressurized simulators also yield a broad range of drop sizes in comparison with drop-formers simulators. The main purpose of this study was to explore in the laboratory the potential of combining spray nozzle simulators with meshes in order to change rainfall characteristics (rainfall intensity and diameters and fall speed of drops). Different types of spray nozzles were tested, such as single full-cone and multiple full-cone nozzles. The impact of the meshes on the simulated rain was studied by testing different materials (i.e. plastic and steel meshes), square apertures and wire thicknesses, and different vertical distances between the nozzle and the meshes underneath. The diameter and fall speed of the rain drops were measured using a Laser Precipitation Monitor (Thies Clima). The rainfall intensity range and coefficients of uniformity of the sprays and the drop size distribution, fall speed and kinetic energy were analysed. Results show that when meshes intercept drop trajectories the spatial distribution of rainfall intensity and the drop size distribution are affected. As the spray nozzles generate typically small drop sizes and narrow drop size distributions, meshes can be used to promote the formation of bigger drops and random their landing positions.

  20. Directional Transport of a Liquid Drop between Parallel-Nonparallel Combinative Plates.

    Science.gov (United States)

    Huang, Yao; Hu, Liang; Chen, Wenyu; Fu, Xin; Ruan, Xiaodong; Xie, Haibo

    2018-04-17

    Liquids confined between two parallel plates can perform the function of transmission, support, or lubrication in many practical applications, due to which to maintain liquids stable within their working area is very important. However, instabilities may lead to the formation of leaking drops outside the bulk liquid, thus it is necessary to transport the detached drops back without overstepping the working area and causing destructive leakage to the system. In this study, we report a novel and facile method to solve this problem by introducing the wedgelike geometry into the parallel gap to form a parallel-nonparallel combinative construction. Transport performances of this structure were investigated. The criterion for self-propelled motion was established, which seemed more difficult to meet than that in the nonparallel gap. Then, we performed a more detailed investigation into the drop dynamics under squeezing and relaxing modes because the drops can surely return in hydrophilic combinative gaps, whereas uncertainties arose in gaps with a weak hydrophobic character. Therefore, through exploration of the transition mechanism of the drop motion state, a crucial factor named turning point was discovered and supposed to be directly related to the final state of the drops. On the basis of the theoretical model of turning point, the criterion to identify whether a liquid drop returns to the parallel part under squeezing and relaxing modes was achieved. These criteria can provide guidance on parameter selection and structural optimization for the combinative gap, so that the destructive leakage in practical productions can be avoided.

  1. Combined discrete nebulization and microextraction process for molybdenum determination by flame atomic absorption spectrometry (FAAS); Avaliacao da combinacao da nebulizacao discreta e processos de microextracao aplicados a determinacao de molibdenio por espectrometria de absorcao atomica com chama (FAAS)

    Energy Technology Data Exchange (ETDEWEB)

    Oviedo, Jenny A.; Jesus, Amanda M.D. de; Fialho, Lucimar L.; Pereira-Filho, Edenir R., E-mail: erpf@ufscar.br [Universidade Federal de Sao Carlos (UFSCar), SP (Brazil). Departamento de Quimica

    2014-04-15

    Simple and sensitive procedures for the extraction/preconcentration of molybdenum based on vortex-assisted solidified floating organic drop microextraction (VA-SFODME) and cloud point combined with flame absorption atomic spectrometry (FAAS) and discrete nebulization were developed. The influence of the discrete nebulization on the sensitivity of the molybdenum preconcentration processes was studied. An injection volume of 200 μ resulted in a lower relative standard deviation with both preconcentration procedures. Enrichment factors of 31 and 67 and limits of detection of 25 and 5 μ L{sup -1} were obtained for cloud point and VA-SFODME, respectively. The developed procedures were applied to the determination of Mo in mineral water and multivitamin samples. (author)

  2. Fully automatic exposed and in-syringe dynamic single-drop microextraction with online agitation for the determination of polycyclic musks in surface waters of the Pearl River Estuary and South China Sea.

    Science.gov (United States)

    Wang, Xiaowei; Yuan, Ke; Liu, Hongtao; Lin, Li; Luan, Tiangang

    2014-07-01

    An automatic exposed and in-syringe dynamic single-drop microextraction method (SDME) for the determination of five polycyclic musks in natural waters was developed using gas chromatography with mass spectrometry. Online agitation was first introduced to the automatic SDME with a magnetic mixer fixed to the bottom of the sample tray of the autosampler. A high enrichment factor (110 ∼182) for the target analytes could be achieved after several parameters that affected the microextraction were optimized. The recoveries were between 84.9 and 119.5%, while the limit of detection ranged from 3.4 to 11 ng/L with relative standard deviation sea waters that were collected from the Pearl River Estuary and the South China Sea. Most polycyclic musks could be detected with the total concentrations ranging from 58.9 to 528.5 ng/L. By using spatial interpolation method of ordinary kriging, the most contaminated area was found near the cities of Dongguan and Guangzhou with local discharge via the major rivers. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Accelerated solvent extraction combined with dispersive liquid-liquid microextraction before gas chromatography with mass spectrometry for the sensitive determination of phenols in soil samples.

    Science.gov (United States)

    Xing, Han-Zhu; Wang, Xia; Chen, Xiang-Feng; Wang, Ming-Lin; Zhao, Ru-Song

    2015-05-01

    A method combining accelerated solvent extraction with dispersive liquid-liquid microextraction was developed for the first time as a sample pretreatment for the rapid analysis of phenols (including phenol, m-cresol, 2,4-dichlorophenol, and 2,4,6-trichlorophenol) in soil samples. In the accelerated solvent extraction procedure, water was used as an extraction solvent, and phenols were extracted from soil samples into water. The dispersive liquid-liquid microextraction technique was then performed on the obtained aqueous solution. Important accelerated solvent extraction and dispersive liquid-liquid microextraction parameters were investigated and optimized. Under optimized conditions, the new method provided wide linearity (6.1-3080 ng/g), low limits of detection (0.06-1.83 ng/g), and excellent reproducibility (extraction with dispersive liquid-liquid microextraction as a sample pretreatment procedure coupled with gas chromatography and mass spectrometry is an excellent method for the rapid analysis of trace levels of phenols in environmental soil samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Dispersive liquid-liquid microextraction based on solidification of floating organic drop for simultaneous separation/preconcentration of nickel, cobalt and copper prior to determination by electrothermal atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Mooud Amirkavei

    2013-01-01

    Full Text Available A dispersive liquid-liquid microextraction based on solidification of floating organic drop for simultaneous extraction of trace amounts of nickel, cobalt and copper followed by their determination with electrothermal atomic absorption spectrometry was developed. 300 µL of acetone and 1-undecanol was injected into an aqueous sample containing diethyldithiocarbamate complexes of metal ions. For a sample volume of 10 mL, enrichment factors of 277, 270 and 300 and detection limits of 1.2, 1.1 and 1 ng L-1 for nickel, cobalt and copper were obtained, respectively. The method was applied to the extraction and determination of these metals in different water samples.

  5. Microvolume turbidimetry for rapid and sensitive determination of the acid labile sulfide fraction in waters after headspace single-drop microextraction with in situ generation of volatile hydrogen sulfide.

    Science.gov (United States)

    Lavilla, I; Pena-Pereira, F; Gil, S; Costas, M; Bendicho, C

    2009-08-04

    In this work, we demonstrate the feasibility of applying headspace single-drop microextraction with in-drop precipitation for the quantitative determination of the acid labile sulfide fraction (H2S, HS-, and S2- (free sulfide), amorphous FeS and some metal sulfide complexes-clusters as ZnS) in aqueous samples by microvolume turbidimetry. The methodology lies in the in situ hydrogen sulfide generation and subsequent sequestration into an alkaline microdrop containing ZnO(2)(2-) and exposed to the headspace above the stirred aqueous sample. The ZnS formed in the drop was then determined by microvolume turbidimetry. The optimum experimental conditions of the proposed method were: 2 microL of a microdrop containing 750 mg L(-1) Zn(II) in 1 mol L(-1) NaOH exposed to the headspace of a 20-mL aqueous sample stirred at 1600 rpm during 80 s after derivatization with 1 mL of 6 mol L(-1) HCl. An enrichment factor of 1710 was achieved in only 80 s. The calibration graph was linear in the range of 5-100 microg L(-1) with a detection limit of 0.5 microg L(-1). The repeatability, expressed as relative standard deviation, was 5.8% (N = 9). Finally, the proposed methodology was successfully applied to the determination of the acid labile sulfide fraction in different natural water samples.

  6. Dispersive liquid-liquid microextraction (DLLME combined with graphite furnace atomic absorption spectrometry (GFAAS for determination of trace Cu and Zn in water Samples

    Directory of Open Access Journals (Sweden)

    Ghorbani A.

    2014-07-01

    Full Text Available Dispersive liquid-liquid microextraction (DLLME combined with graphite furnace atomic absorption spectrometry (GFAAS was proposed for the determination of trace amounts of Copper and Zinc ions using 8-hydroxyquinoline (8-HQ as chelating agent. Several factors influencing the microextraction efficiency of Cu and Zn and their subsequent determinations, such as pH, extraction and disperser solvent type and their volume, concentration of the chelating agent and extraction time were studied, and the optimized experimental conditions were established. After extraction, the enrichment factors were 25 and 26 for Cu and Zn, respectively. The detection limits of the method were 0.025 and 0.0033 μg/L for Cu and Zn, and the relative standard deviations (R.S.D for five determinations of 1 ng/ml Cu and Zn were 8.51% and 7.41%, respectively.

  7. Liquid phase microextraction strategies combined with total reflection X-ray spectrometry for the determination of low amounts of inorganic antimony species in waters.

    Science.gov (United States)

    Marguí, Eva; Sagué, Marta; Queralt, Ignasi; Hidalgo, Manuela

    2013-07-05

    In the present study, and taking into account the microanalytical capability of total reflection X-ray spectrometry (TXRF), we explored the possibilities of hollow fibre liquid-phase microextraction (HF-LPME) and dispersive liquid-liquid microextraction (DLLME) combined with TXRF for the determination of low amounts of inorganic Sb species in waters. For each of the LPME configurations aforementioned, experimental parameters affecting Sb extraction but specially the proper sample preparation process (deposition volume on the reflective carrier and drying mode) and measurement conditions for subsequent TXRF analysis have been carefully evaluated. The best analytical strategy for the determination of Sb(III) and Sb(V) in the low μg L(-1) range was found to be the application of the DLLME mode before TXRF analysis. The developed methodology was successfully applied to the determination of inorganic Sb speciation in different types of spiked water samples. Copyright © 2013 Elsevier B.V. All rights reserved.

  8. Hollow fiber-liquid phase microextraction combined with gas chromatography for the determination of phenothiazine drugs in urine.

    Science.gov (United States)

    Xiao, Qin; Hu, Bin

    2010-06-01

    A simple method of hollow fiber-liquid phase microextraction (HF-LPME) combined with gas chromatography (GC) was developed for the analysis of four phenothiazine drugs (promethazine, promazine, chlorpromazine and trifluoperazine) in human urine samples. All variables affecting the extraction of target analytes including organic solvent type, stirring rate, extraction time, extraction temperature, pH of sample solution and ionic strength were carefully studied and optimized. Under the optimal conditions, the analytical performance of HF-LPME-GC-flame photometric detector (FPD) and HF-LPME-GC-flame ionization detector (FID) were evaluated and compared. The results showed that the HF-LPME-GC-FID was more sensitive than HF-LPME-GC-FPD for the determination of four target phenothiazine drugs, while the signal peak shape and resolution obtained by HF-LPME-GC-FPD was better than that obtained by HF-LPME-GC-FID. HF-LPME-GC-FPD/FID was successfully applied for the assay of the interested phenothiazine drugs in urine sample, and the excretion of the drugs was also investigated by monitoring the variation of the concentration of chlorpromazine in urine of a psychopath within 8 h after drug-taking. The proposed method provided an effective and fast way for the therapeutic drug monitoring (TDM) of phenothiazine. Copyright 2010 Elsevier B.V. All rights reserved.

  9. Ligandless, ion pair-based and ultrasound assisted emulsification solidified floating organic drop microextraction for simultaneous preconcentration of ultra-trace amounts of gold and thallium and determination by GFAAS.

    Science.gov (United States)

    Fazelirad, Hamid; Taher, Mohammad Ali

    2013-01-15

    In the present work, a new, simple and efficient method for simultaneous preconcentration of ultra-trace amounts of gold and thallium is developed using an ion pair based-ultrasound assisted emulsification-solidified floating organic drop microextraction procedure before graphite furnace atomic absorption spectrometry determination. This methodology was used to preconcentrate the ion pairs formed between AuCl(4)(-) and TlCl(4)(-) and [C(23)H(42)]N(+) in a microliter-range volume of 1-undecanol. Several factors affecting the microextraction efficiency, such as HCl volume, type and volume of extraction solvent, sonication time, sample volume, temperature, ionic strength and [C(23)H(42)]NCl volume were investigated and optimized. Under the optimized conditions, the enrichment factor of 441 and 443 and calibration graphs of 2.2-89 and 22.2-667 ng L(-1) for gold and thallium were obtained, respectively. The intra- and inter-day precision of ± 4.4 and ± 4.9% for Au and ± 4.8 and ± 5.4% for Tl were obtained. The detection limit was 0.66 ng L(-1) for Au and 4.67 ng L(-1) for Tl. The results show that the liquid-liquid pretreatment using ion pair forming, is sensitive, rapid, simple and safe method for the simultaneous preconcentration of gold and thallium. The method was successfully applied for determination of gold and thallium in natural water and hair samples. Copyright © 2012 Elsevier B.V. All rights reserved.

  10. Applications of Liquid-Phase Microextraction in the Sample Preparation of Environmental Solid Samples

    Directory of Open Access Journals (Sweden)

    Helena Prosen

    2014-05-01

    Full Text Available Solvent extraction remains one of the fundamental sample preparation techniques in the analysis of environmental solid samples, but organic solvents are toxic and environmentally harmful, therefore one of the possible greening directions is its miniaturization. The present review covers the relevant research from the field of application of microextraction to the sample preparation of environmental solid samples (soil, sediments, sewage sludge, dust etc. published in the last decade. Several innovative liquid-phase microextraction (LPME techniques that have emerged recently have also been applied as an aid in sample preparation of these samples: single-drop microextraction (SDME, hollow fiber-liquid phase microextraction (HF-LPME, dispersive liquid-liquid microextraction (DLLME. Besides the common organic solvents, surfactants and ionic liquids are also used. However, these techniques have to be combined with another technique to release the analytes from the solid sample into an aqueous solution. In the present review, the published methods were categorized into three groups: LPME in combination with a conventional solvent extraction; LPME in combination with an environmentally friendly extraction; LPME without previous extraction. The applicability of these approaches to the sample preparation for the determination of pollutants in solid environmental samples is discussed, with emphasis on their strengths, weak points and environmental impact.

  11. Applications of liquid-phase microextraction in the sample preparation of environmental solid samples.

    Science.gov (United States)

    Prosen, Helena

    2014-05-23

    Solvent extraction remains one of the fundamental sample preparation techniques in the analysis of environmental solid samples, but organic solvents are toxic and environmentally harmful, therefore one of the possible greening directions is its miniaturization. The present review covers the relevant research from the field of application of microextraction to the sample preparation of environmental solid samples (soil, sediments, sewage sludge, dust etc.) published in the last decade. Several innovative liquid-phase microextraction (LPME) techniques that have emerged recently have also been applied as an aid in sample preparation of these samples: single-drop microextraction (SDME), hollow fiber-liquid phase microextraction (HF-LPME), dispersive liquid-liquid microextraction (DLLME). Besides the common organic solvents, surfactants and ionic liquids are also used. However, these techniques have to be combined with another technique to release the analytes from the solid sample into an aqueous solution. In the present review, the published methods were categorized into three groups: LPME in combination with a conventional solvent extraction; LPME in combination with an environmentally friendly extraction; LPME without previous extraction. The applicability of these approaches to the sample preparation for the determination of pollutants in solid environmental samples is discussed, with emphasis on their strengths, weak points and environmental impact.

  12. Rapid analysis of aflatoxins B1, B2, and ochratoxin A in rice samples using dispersive liquid-liquid microextraction combined with HPLC.

    Science.gov (United States)

    Lai, Xian-Wen; Sun, Dai-Li; Ruan, Chun-Qiang; Zhang, He; Liu, Cheng-Lan

    2014-01-01

    A novel, simple, and rapid method is presented for the analysis of aflatoxin B1, aflatoxin B2, and ochratoxin A in rice samples by dispersive liquid-liquid microextraction combined with LC and fluorescence detection. After extraction of the rice samples with a mixture of acetonitrile/water/acetic acid, mycotoxins were rapidly partitioned into a small volume of organic solvent (chloroform) by dispersive liquid-liquid microextraction. The three mycotoxins were simultaneously determined by LC with fluorescence detection after precolumn derivatization for aflatoxin B1 and B2. Parameters affecting both extraction and dispersive liquid-liquid microextraction procedures, including the extraction solvent, the type and volume of extractant, the volume of dispersive solvent, the addition of salt, the pH and the extraction time, were optimized. The optimized protocol provided an enrichment factor of approximately 1.25 and with detection of limits (0.06-0.5 μg/kg) below the maximum levels imposed by current regulations for aflatoxins and ochratoxin A. The mean recovery of three mycotoxins ranged from 82.9-112%, with a RSD less than 7.9% in all cases. The method was successfully applied to measure mycotoxins in commercial rice samples collected from local supermarkets in China. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Determination of ten pyrethroids in various fruit juices: comparison of dispersive liquid-liquid microextraction sample preparation and QuEChERS method combined with dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Zhang, Yaohai; Zhang, Xuelian; Jiao, Bining

    2014-09-15

    Dispersive liquid-liquid microextraction (DLLME) sample preparation and the quick, easy, cheap, effective, rugged and safe (QuEChERS) method combined with DLLME were developed and compared for the analysis of ten pyrethroids in various fruit juices using gas chromatography-electron capture detection (GC-ECD). QuEChERS-DLLME method has found its widespread applications to all the fruit juices including those samples with more complex matrices (orange, lemon, kiwi and mango) while DLLME was confined to the fruit juices with simpler matrices (apple, pear, grape and peach). The two methods provided acceptable recoveries and repeatability. In addition, the applicabilities of two methods were demonstrated with the real samples and further confirmed by gas chromatography-mass spectrometry (GC-MS). Copyright © 2014. Published by Elsevier Ltd.

  14. Feasibility of using Lokomat combined with functional electrical stimulation for the rehabilitation of foot drop

    Directory of Open Access Journals (Sweden)

    Christian B. Laursen

    2016-08-01

    Full Text Available This study investigated the clinical feasibility of combining the electromechanical gait trainer Lokomat with functional electrical therapy (LokoFET, stimulating the common peroneal nerve during the swing phase of the gait cycle to correct foot drop as an integrated part of gait therapy. Five patients with different acquired brain injuries trained with LokoFET 2-3 times a week for 3-4 weeks. Pre- and post-intervention evaluations were performed to quantify neurophysiological changes related to the patients’ foot drop impairment during the swing phase of the gait cycle. A semi-structured interview was used to investigate the therapists’ acceptance of LokoFET in clinical practice. The patients showed a significant increase in the level of activation of the tibialis anterior muscle and the maximal dorsiflexion during the swing phase, when comparing the pre- and post-intervention evaluations. This showed an improvement of function related to the foot drop impairment. The interview revealed that the therapists perceived the combined system as a useful tool in the rehabilitation of gait. However, lack of muscle selectivity relating to the FES element of LokoFET was assessed to be critical for acceptance in clinical practice.

  15. Two-step microextraction combined with high performance liquid chromatographic analysis of pyrethroids in water and vegetable samples.

    Science.gov (United States)

    Mukdasai, Siriboon; Thomas, Chunpen; Srijaranai, Supalax

    2014-03-01

    Dispersive liquid microextraction (DLME) combined with dispersive µ-solid phase extraction (D-µ-SPE) has been developed as a new approach for the extraction of four pyrethroids (tetramethrin, fenpropathrin, deltamethrin and permethrin) prior to the analysis by high performance liquid chromatography (HPLC) with UV detection. 1-Octanol was used as the extraction solvent in DLME. Magnetic nanoparticles (Fe3O4) functionalized with 3-aminopropyl triethoxysilane (APTS) were used as the dispersive in DLME and as the adsorbent in D-µ-SPE. The extracted pyrethroids were separated within 30 min using isocratic elution with acetonitrile:water (72:28). The factors affecting the extraction efficiency were investigated. Under the optimum conditions, the enrichment factors were in the range of 51-108. Linearity was obtained in the range 0.5-400 ng mL(-1) (tetramethrin) and 5-400 ng mL(-1) (fenpropathrin, deltamethrin and permethrin) with the correlation coefficients (R(2)) greater than 0.995. Detection limits were 0.05-2 ng mL(-1) (water samples) and 0.02-2.0 ng g(-1) (vegetable samples). The relative standard deviations of peak area varied from 1.8 to 2.5% (n=10). The extraction recoveries of the four pyrethroids in field water and vegetable samples were 91.7-104.5%. The proposed method has high potential for use as a sensitive method for determination of pyrethroid residues in water and vegetable samples. Copyright © 2013 Elsevier B.V. All rights reserved.

  16. The effect of surfactant on headspace single drop microextraction for the determination of some volatile aroma compounds in citronella grass and lemongrass leaves by gas chromatography

    Science.gov (United States)

    A rapid method for the determination of some volatile aromatic compounds (VACs), including citronellal, citronellol, neral, geranial, geraniol, and eugenol in citronella grass and lemongrass leaves, was developed using surfactant as a surface tension modifier while performing headspace single drop m...

  17. Methods of liquid phase microextraction for the determination of cadmium in environmental samples.

    Science.gov (United States)

    Pires Santos, Analú; das Graças Andrade Korn, Maria; Azevedo Lemos, Valfredo

    2017-08-09

    Liquid phase microextraction (LPME) has been widely used in extraction and preconcentration systems as an excellent alternative to conventional liquid phase extraction. In this work, a critical review is presented on liquid phase microextraction techniques used in the determination of cadmium in environmental samples. LPME techniques are classified into three main groups: single-drop liquid phase microextraction (SDME), hollow fiber liquid phase microextraction (HF-LPME), and dispersive liquid-liquid microextraction (DLLME). Methods involving these liquid phase microextraction techniques are described, addressing advantages and disadvantages, samples, figures of merit, and trends.

  18. Optimization of a methodology for the simultaneous determination of deltamethrin, permethrin and malathion in stored wheat samples using dispersive liquid-liquid microextraction with solidification of floating organic drop and HPLC-UV.

    Science.gov (United States)

    Pirsaheb, Meghdad; Rezaei, Mansour; Fattahi, Nazir; Karami, Mohammad; Sharafi, Kiomars; Ghaffari, Hamid R

    2017-09-02

    The purpose of this study was to investigate common pesticides in stored wheat at Kermanshah province's silos in Iran. A simple, inexpensive, reliable and environmentally friendly method based on dispersive liquid-liquid microextraction with solidification of floating organic drop was developed. The analytical characteristics of the method were determined. Also, various parameters such as the materials of the silos, types of ownerships of the silos, geographic orientation of silo locations and climatic conditions of silo locations on pesticide residues in studied wheat samples were investigated. Among all the studied parameters, the climatic conditions of silo locations showed the highest influence on pesticide residues in wheat samples. Generally, 61.2% of the samples had pesticide levels below the method detection limits and 38.8% of the total samples had at least one of the understudied pesticides. Also, 13.9% of the samples had deltamethrin residues, 16.7% of the samples had permethrin, 22.2% of the samples had malathion, 11.1% of the samples had both permethrin and malathion and 2.8% of the samples had both deltamethrin and malathion. The results revealed that the residues of deltamethrin and malathion were lower than the standard level announced by European Union regulation and only three samples contained permethrin higher than Europe standard level.

  19. Photoassisted vapor generation in the presence of organic acids for ultrasensitive determination of Se by electrothermal-atomic absorption spectrometry following headspace single-drop microextraction

    International Nuclear Information System (INIS)

    Figueroa, Raul; Garcia, Monica; Lavilla, Isela; Bendicho, Carlos

    2005-01-01

    A method is described for the determination of selenium at the pg/mL level by electrothermal-atomic absorption spectrometry using in situ photogeneration of Se vapors, headspace sequestration onto an aqueous microdrop containing Pd(II) and subsequent injection in a graphite tube. Several organic acids (formic, oxalic, acetic, citric and ethylenediaminetetraacetic) have been tried for photoreduction of Se(IV) into volatile Se compounds under UV irradiation. Experimental variables such as UV irradiation time, organic acid concentration, Pd(II) concentration in the drop, sample and drop volumes, extraction time and pH were fully optimized. Low-molecular weight acids such as formic and acetic provided optimal photogeneration of volatile Se species at a 0.6 mol/L concentration. Citric and ethylenediaminetetraacetic acid allowed to use a concentration as low as 1 mmol/L, but extraction times were longer than for formic and acetic acids. Photogeneration of (CH 3 ) 2 Se from Se(IV) in the presence of acetic acid provided a detection limit of 20 pg/mL, a preconcentration factor of nearly 285 and a precision, expressed as relative standard deviation, of 4%. Analytical performance seemed to depend not only on the photogeneration efficiency obtained with each acid but also on the stability of the vapors in the headspace. The method showed a high freedom from interferences caused by saline matrices, but interferences were observed for transition metals at a relatively low concentration

  20. Simple method for the determination of personal care product ingredients in lettuce by ultrasound-assisted extraction combined with solid-phase microextraction followed by GC-MS.

    Science.gov (United States)

    Cabrera-Peralta, Jerónimo; Peña-Alvarez, Araceli

    2018-02-19

    A simple method for the simultaneous determination of personal care product ingredients: galaxolide, tonalide, oxybenzone, 4-methylbenzyliden camphor, padimate-o, 2-ethylhexyl methoxycinnamate, octocrylene, triclosan, and methyl triclosan in lettuce by ultrasound-assisted extraction combined with solid-phase microextraction followed by gas chromatography with mass spectrometry was developed. Lettuce was directly extracted by ultrasound-assisted extraction with methanol, this extract was combined with water, extracted by solid-phase microextraction in immersion mode, and analyzed by gas chromatography with mass spectrometry. Good linear relationships (25-250 ng/g, R 2  > 0.9702) and low detection limits (1.0-25 ng/g) were obtained for analytes along with acceptable precision for almost all analytes (RSDs < 20%). The validated method was applied for the determination of personal care product ingredients in commercial lettuce and lettuces grown in soil and irrigated with the analytes, identifying the target analytes in leaves and roots of the latter. This procedure is a miniaturized and environmentally friendly proposal which can be a useful tool for quality analysis in lettuce. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Analysis of chlorpheniramine in human urine samples using dispersive liquid-liquid microextraction combined with high-performance liquid chromatography

    Directory of Open Access Journals (Sweden)

    Mehdi Maham

    2014-09-01

    Full Text Available A simple and environmentally friendly microextraction technique was used for determination of chlorpheniramine (CPM, an antihistamine drug, in human urine samples using dispersive liquid-liquid microextraction (DLLME followed by high performance liquid chromatography with diode array detection (HPLC-DAD. In this extraction technique, an appropriate mixture of acetonitrile (disperser solvent and carbon tetrachloride (extraction solvent was rapidly injected into the urine sample containing the target analyte. Tiny droplets of extractant were formed and dispersed into the sample solution and then sedimented at the bottom of the conical test tube by centrifugation. Under optimal conditions, the calibration curve was linear in the range of 0.055-5.5 µg mL-1, with a detection limit of 16.5 ng mL-1. This proposed method was successfully applied to the analysis of real urine samples. Low consumption of toxic organic solvents, simplicity of operation, low cost and acceptable figures of merit are the main advantages of the proposed technique.

  2. Combined microextraction by packed sorbent and high-performance liquid chromatography-ultraviolet detection for rapid analysis of ractopamine in porcine muscle and urine samples.

    Science.gov (United States)

    Du, Wei; Zhao, Gang; Fu, Qiang; Sun, Min; Zhou, Huiyan; Chang, Chun

    2014-02-15

    A method for rapid analysis of ractopamine in porcine muscle and urine was developed and validated. The method was based on combined of microextraction by packed sorbent (MEPS) and high-performance liquid chromatography with ultraviolet detection (HPLC-UV). Parameters of the MEPS procedure affecting extraction efficiency were optimised. Optimum extraction conditions were 100 μL of sample in five extraction cycles and sampling time of 0.9985). Accuracies of muscle and urine analyses were 93.9-109.2% and 93.4-105.1%, respectively. Intra-day and inter-day precisions (RSD%) were lower than 11.8% for both analyses. The method was applied for rapid analysis of ractopamine in biological samples. The method was simpler and could be used to screen other β₂-agonists in other extraction media. Copyright © 2013 Elsevier Ltd. All rights reserved.

  3. Maghemite nanoparticle-decorated hollow fiber electromembrane extraction combined with dispersive liquid-liquid microextraction for the determination of thymol from Carum copticum

    DEFF Research Database (Denmark)

    Khajeh, Mostafa; Pedersen-Bjergaard, Stig; Bohlooli, Mousa

    2017-01-01

    BACKGROUND A novel technique using maghemite nanoparticle-decorated hollow fibers to assist electromembrane extraction is proposed. Electromembrane extraction combined with dispersive liquid–liquid microextraction (EME-DLLME) was applied for the extraction of thymol from Carum copticum, followed...... by gas chromatography with flame ionization detection (GC-FID). RESULTS The use of maghemite nanoparticle-decorated hollow fibers was found to improve the extraction efficiency of thymol significantly. Important operational parameters, including pH of acceptor phase, extraction time, voltage.......2% respectively. The intra- and inter-day accuracy was higher than 93.6%. CONCLUSION The results indicated that EME-DLLME/GC-FID is a useful technique for the extraction and determination of thymol in C copticum. © 2016 Society of Chemical Industry...

  4. Combination of electromembrane extraction and liquid-phase microextraction in a single step: Simultaneous group separation of acidic and basic drugs

    DEFF Research Database (Denmark)

    Huang, Chuixiu; Seip, Knut Fredrik; Gjelstad, Astrid

    2015-01-01

    Electromembrane extraction (EME) and liquid-phase microextraction (LPME) were combined in a single step for the first time to realize simultaneous and clear group separation of basic and acidic drugs. Using 2-nitrophenyl octyl ether as the supported liquid membrane (SLM) for EME and dihexyl ether...... as the SLM for LPME, basic and acidic drugs were extracted and separated simultaneously from a low pH sample by EME and LPME, respectively. After 15 min of extraction, basic drugs (citalopram and sertraline) were exhaustively extracted, whereas the recoveries for acidic drugs (ketoprofen and ibuprofen) were...... in the range of 76%-86%. Longer extraction time provided higher recoveries for the acidic drugs, but this somewhat deteriorated the group separation. Matrices effects from the coexisting acidic drugs/basic drugs were tested, and we observed that simultaneous EME/LPME was not affected by coexisting drugs...

  5. In situ growth of IRMOF-3 combined with ionic liquids to prepare solid-phase microextraction fibers.

    Science.gov (United States)

    Zheng, Juan; Li, Siyan; Wang, Ying; Li, Lei; Su, Chengyong; Liu, Hong; Zhu, Fang; Jiang, Ruifen; Ouyang, Gangfeng

    2014-06-04

    A superior solid-phase microextraction (SPME) fiber-coating material, IRMOF-3@ILs/PDMS, was prepared by the in situ growth of IRMOF-3 onto stainless-steel wires and protection with ionic liquids (ILs) and polydimethylsiloxane (PDMS). The ILs can efficiently prevent the substantial cracking of IRMOF-3 caused by moisture, and a thin PDMS film can protect the IRMOF-3@ILs material to achieve a much better extraction efficiency as well as excellent resistance to high temperature and high humidity. This IRMOF-3@ILs/PDMS coating possessed a porous structure, a rough surface and an increased lifespan (by at least 100 times) compared with that of IRMOF-3. The coating was evaluated by analyzing four polycyclic aromatic hydrocarbons (PAHs) in water, and good precision (analysis of PAHs in rainwater by coupling it with gas chromatography-mass spectrometry (GC-MS). Copyright © 2014 Elsevier B.V. All rights reserved.

  6. Risk identification for quality on stage of pharmaceutical development of combined eye drops for glaucoma treatment

    Directory of Open Access Journals (Sweden)

    Олександр Миколайович Якубчук

    2015-12-01

    Full Text Available Aim: To identify the possible risks associated with critical quality attribute of combined eye drops for the treatment of glaucoma using of common risk evaluation methodologies for plannig a drug quality on the stage of pharmaceutical development. Methods: The paper used method of causal analysis. The maximal number of factors has been define to identify potential factors that provide most significant impact on the drug quality and Ishikawa diagram - graphical representation of causes and effects has been built.Results: Analysis allowed to organize the possible factors affecting the drug quality in the generalized categories: quality control methods, medicines and excipients, primary packaging, proper manufacturing conditions and the stage of the process. The most important factors that are carriers of the risk factors and may lead to negative effects have been identified for the generalized categories.Conclusions: Determined at the stage of pharmaceutical development potential critical quality attribute of AFI, excipients and primary packaging, critical parameters of the process, provide a better understanding, reduction and adoption of risk in subsequent stages of the life cycle of the drug

  7. Hollow fiber liquid phase microextraction combined with electrothermal atomic absorption spectrometry for the speciation of arsenic (III) and arsenic (V) in fresh waters and human hair extracts

    Energy Technology Data Exchange (ETDEWEB)

    Jiang Hongmei [Department of Chemistry, Wuhan University, Wuhan 430072 (China); Hu Bin [Department of Chemistry, Wuhan University, Wuhan 430072 (China)], E-mail: binhu@whu.edu.cn; Chen Beibei; Xia Linbo [Department of Chemistry, Wuhan University, Wuhan 430072 (China)

    2009-02-16

    A new method of hollow fiber liquid phase microextraction (HF-LPME) using ammonium pyrrolidine dithiocarbamate (APDC) as extractant combined with electrothermal atomic absorption spectrometry (ETAAS) using Pd as permanent modifier has been described for the speciation of As(III) and As(V). In a pH range of 3.0-4.0, the complex of As(III)-APDC complex can be extracted using toluene as the extraction solvent leaving As(V) in the aqueous layer. The post extraction organic phase was directly injected into ETAAS for the determination of As(III). To determine total arsenic in the samples, first As(V) was reduced to As(III) by L-cysteine, and then a microextraction method was performed prior to the determination of total arsenic. As(V) assay was based on subtracting As(III) form the total arsenic. All parameters, such as pH of solution, type of organic solvent, the amount of APDC, stirring rate and extraction time, affecting the separation of As(III) from As(V) and the extraction efficiency of As(III) were investigated, and the optimized extraction conditions were established. Under optimized conditions, a detection limit of 0.12 ng mL{sup -1} with enrichment factor of 78 was achieved. The relative standard deviation (R.S.D.) of the method for five replicate determinations of 5 ng mL{sup -1} As(III) was 8%. The developed method was applied to the speciation of As(III) and As(V) in fresh water and human hair extracts, and the recoveries for the spiked samples are 86-109%. In order to validate the developed method, three certified reference materials such as GBW07601 human hair, BW3209 and BW3210 environmental water were analyzed, and the results obtained were in good agreement with the certified values provided.

  8. Direct solid phase microextraction combined with gas chromatography - Mass spectrometry for the determination of biogenic amines in wine.

    Science.gov (United States)

    Papageorgiou, Myrsini; Lambropoulou, Dimitra; Morrison, Calum; Namieśnik, Jacek; Płotka-Wasylka, Justyna

    2018-06-01

    A direct method based on immersion solid phase microextraction (DI-SPME) gas chromatography mass-spectrometry (GC-MS) was optimized and validated for the determination of 16 biogenic amines in Polish wines. In the analysis two internal standards were used: 1,7-diaminoheptane and bis-3-aminopropylamine. The method allows for simultaneous extraction and derivatization, providing a simple and fast mode of extraction and enrichment. Different parameters which affect the extraction procedure were studied and optimized including ionic strength (0-25%), fiber materials (PDMS/DVB, PDMS/DVD + OC, Polyacrylate, Carboxen/PDMS and DVB/CAR/PDMS) and timings of the extraction, derivatization and desorption processes. Validation studies confirmed the linearity, sensitivity, precision and accuracy of the method. The method was successfully applied to the analysis of 44 wine samples originating from several regions of Poland and 3 wine samples from other countries. Analysis showed that many of the samples contained all examined biogenic amines. The method, assessed using an Eco-Scale tool with satisfactory results, was found to be green in terms of hazardous chemicals and solvents usage, energy consumption and production of waste. Therefore the proposed method can be safely used in the wine industry for routine analysis of BAs in wine samples with a minimal detrimental impact on human health and the environment. Copyright © 2018 Elsevier B.V. All rights reserved.

  9. Combination of liquid-phase hollow fiber membrane microextraction with gas chromatography-negative chemical ionization mass spectrometry for the determination of dichlorophenol isomers in water and urine.

    Science.gov (United States)

    Lai, Bin-Wei; Liu, Bo-Min; Malik, Pradip K; Wu, Hui-Fen

    2006-08-18

    A method for the determination of trace amount of dichlorophenol isomers in urine samples using the combination of liquid-phase hollow fiber microextraction (LPME-HF) with gas chromatography-negative chemical ionization mass spectrometry (GC-NCI-MS) has been demonstrated. The method has been optimized with respect to several parameters including the effects of negative chemical ionization (NCI) reagent pressure, the hollow fiber length, extraction time, stirring rate, sample pH and salt concentration for the determination of dichlorophenol isomers in water. The correlation coefficient (r2) of the calibration curves for 2,5-dichlorophenol, 2,3-dichlorophenol, 2,6-dichlorophenol, 3,5-dichlorophenol and 3,4-dichlorophenol were 0.988, 0.981, 0.985, 0.971 and 0.994, respectively. The average recovery rates for 2,5-dichlorophenol, 2,3-dichlorophenol, 2,6-dichlorophenol, 3,5-dichlorophenol and 3,4-dichlorophenol were 0.97, 0.93, 0.96, 0.95 and 0.95, respectively (n=3 for each dichlorophenol) indicate that the methodology is feasible for the determination of trace amounts of dichlorophenol isomers in water and urine samples. Limits of detection (LOD) have been found to be in the range of 5-20 ng/ml. In addition, differentiation of the five dichlorophenol isomers is an easy task using the current approach of combining LPME-HF with NCI-GC-MS technique since they exhibit different NCI spectra.

  10. Determination of carbohydrates in tobacco by pressurized liquid extraction combined with a novel ultrasound-assisted dispersive liquid-liquid microextraction method.

    Science.gov (United States)

    Cai, Kai; Hu, Deyu; Lei, Bo; Zhao, Huina; Pan, Wenjie; Song, Baoan

    2015-07-02

    A novel derivatization-ultrasonic assisted-dispersive liquid-liquid microextraction (UA-DLLME) method for the simultaneous determination of 11 main carbohydrates in tobacco has been developed. The combined method involves pressurized liquid extraction (PLE), derivatization, and UA-DLLME, followed by the analysis of the main carbohydrates with a gas chromatography-flame ionization detector (GC-FID). First, the PLE conditions were optimized using a univariate approach. Then, the derivatization methods were properly compared and optimized. The aldononitrile acetate method combined with the O-methoxyoxime-trimethylsilyl method was used for derivatization. Finally, the critical variables affecting the UA-DLLME extraction efficiency were searched using fractional factorial design (FFD) and further optimized using Doehlert design (DD) of the response surface methodology. The optimum conditions were found to be 44 μL for CHCl3, 2.3 mL for H2O, 11% w/v for NaCl, 5 min for the extraction time and 5 min for the centrifugation time. Under the optimized experimental conditions, the detection limit of the method (LODs) and linear correlation coefficient were found to be in the range of 0.06-0.90 μg mL(-1) and 0.9987-0.9999. The proposed method was successfully employed to analyze three flue-cured tobacco cultivars, among which the main carbohydrate concentrations were found to be very different. Copyright © 2015 Elsevier B.V. All rights reserved.

  11. Combination of electromembrane extraction with dispersive liquid-liquid microextraction followed by gas chromatographic analysis as a fast and sensitive technique for determination of tricyclic antidepressants.

    Science.gov (United States)

    Seidi, Shahram; Yamini, Yadollah; Rezazadeh, Maryam

    2013-01-15

    For the first time, combination of electromembrane extraction (EME) and dispersive liquid-liquid microextraction (DLLME) followed by gas chromatography-flame ionization detection (GC/FID) was developed for determination of tricyclic antidepressants (TCAs) in untreated human plasma and urine samples. Response surface methodology (RSM) was used for optimization of experimental parameters, so that extraction time of 14min, voltage of 240V, donor phase of 64mM HCl and acceptor phase of 100mM HCl were obtained as optimal extraction conditions. Matrix effect and carry-over were investigated in this work. The results indicated matrix effect for urine and plasma samples in comparison with neat solutions, so match matrix method was used for drawing working calibration curves. However, no carry-over was appeared at the retention time of investigated TCAs (S/N86.5%. The results showed that EME-DLLME-GC/FID is a promising combination for analysis of TCAs present at low concentrations in biological matrices. Copyright © 2012 Elsevier B.V. All rights reserved.

  12. Magnetic silica nanomaterials for solid-phase extraction combined with dispersive liquid-liquid microextraction of ultra-trace quantities of plasticizers

    International Nuclear Information System (INIS)

    Yamini, Yadollah; Faraji, Mohammad; Adeli, Mahnaz

    2015-01-01

    We are presenting surface modified magnetic silica nanoparticles (m-Si-NPs) for use in solid-phase extraction combined with dispersive liquid-liquid microextraction (DLLME). The m-Si-NPs were surface-functionalized with octadecyl groups to give a material for the extraction of the plasticizers dibutyl phthalate, di(2-ethylhexyl) adipate and di(2-ethylhexyl) phthalate from water samples. The functionalized m-Si-NPs were characterized by scanning electron microscopy, FTIR spectroscopy, thermal gravimetric analysis, and vibrating sample magnetometry. The results showed that the m-Si-NPs were well functionalized with octadecyl groups. The effects of various experimental variables on the extraction efficiencies were investigated. The analytes were quantified by GC/FID. Under optimal conditions, the calibration plots are linear in the range from 0.01 to 100 μg∙L -1 , and very high enrichment factors (mean value ∼20,000) were obtained. As a result of the high enrichment factors, the detection limits are as low as 2–3 ng∙L -1 . The method was successfully employed to the extraction of the plasticizers from (spiked) water samples, and recoveries are in the order of 93.9 to 106.7 %. The method is low cost, fast, and very sensitive (author)

  13. Combined solid-phase microextraction and high-performance liquid chromatography with ultroviolet detection for simultaneous analysis of clenbuterol, salbutamol and ractopamine in pig samples.

    Science.gov (United States)

    Du, Wei; Zhang, Siruo; Fu, Qiang; Zhao, Gang; Chang, Chun

    2013-12-01

    A simple and sensitive method based on the combination of solid-phase microextraction (SPME) and high-performance liquid chromatography with ultroviolet detection was developed for the simultaneous determination of clenbuterol, salbutamol and ractopamine in pig samples. Parameters of the SPME procedure affecting extraction efficiency, such as the type of fiber, extraction time, extraction temperature, ion strength, pH of sample and stirring rate, were optimized. The developed method was validated according to the International Conference on Harmonization guidelines. The calibration curves were linear over a range of 0.5-50 µg/L for clenbuterol and ractopamine, and 0.2-20 µg/L for salbutamol. The limits of detection were 0.1 µg/L for clenbuterol, 0.05 µg/L for salbutamol and 0.1 μg/L for ractopamine, respectively. The averages of intra- and inter-day accuracy ranged from 79.8 to 92.4%. The intra-day and inter-day precision were below 9.6% for the three analytes. This method exhibited the advantages of simplicity, rapidity and low solvent consumption, and was suitable for the monitoring of β2 -agonists residue in pig samples. Copyright © 2013 John Wiley & Sons, Ltd.

  14. Solid phase microextraction of diclofenac using molecularly imprinted polymer sorbent in hollow fiber combined with fiber optic-linear array spectrophotometry

    Science.gov (United States)

    Pebdani, Arezou Amiri; Shabani, Ali Mohammad Haji; Dadfarnia, Shayessteh; Khodadoust, Saeid

    2015-08-01

    A simple solid phase microextraction method based on molecularly imprinted polymer sorbent in the hollow fiber (MIP-HF-SPME) combined with fiber optic-linear array spectrophotometer has been applied for the extraction and determination of diclofenac in environmental and biological samples. The effects of different parameters such as pH, times of extraction, type and volume of the organic solvent, stirring rate and donor phase volume on the extraction efficiency of the diclofenac were investigated and optimized. Under the optimal conditions, the calibration graph was linear (r2 = 0.998) in the range of 3.0-85.0 μg L-1 with a detection limit of 0.7 μg L-1 for preconcentration of 25.0 mL of the sample and the relative standard deviation (n = 6) less than 5%. This method was applied successfully for the extraction and determination of diclofenac in different matrices (water, urine and plasma) and accuracy was examined through the recovery experiments.

  15. Polymer monolithic capillary microextraction combined on-line with inductively coupled plasma MS for the determination of trace rare earth elements in biological samples.

    Science.gov (United States)

    Zhang, Lin; Chen, Beibei; He, Man; Hu, Bin

    2013-07-01

    A rapid and sensitive method based on polymer monolithic capillary microextraction combined on-line with microconcentric nebulization inductively coupled plasma MS has been developed for the determination of trace/ultratrace rare earth elements in biological samples. For this purpose, the iminodiacetic acid modified poly(glycidyl methacrylate-trimethylolpropane trimethacrylate) monolithic capillary was prepared and characterized by SEM and FTIR spectroscopy. Factors affecting the extraction efficiency, such as sample pH, sample flow rate, sample/eluent volume, and coexisting ions were investigated in detail. Under the optimal conditions, the LODs for rare earth elements were in the range of 0.08 (Er) to 0.97 ng/L (Nd) with a sampling frequency of 8.5 h(-1), and the RSDs were between 1.5% (Sm) and 7.4% (Nd) (c = 20 ng/L, n = 7). The proposed method was successfully applied to the analysis of trace/ultratrace rare earth elements in human urine and serum samples, and the recoveries for the spiked samples were in the range of 82-105%. The developed method was simple, rapid, sensitive, and favorable for the analysis of trace/ultratrace rare earth elements in biological samples with limited sample volume. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Dispersive Liquid-Liquid Microextraction Combined with Ultrahigh Performance Liquid Chromatography/Tandem Mass Spectrometry for Determination of Organophosphate Esters in Aqueous Samples

    Directory of Open Access Journals (Sweden)

    Haiying Luo

    2014-01-01

    Full Text Available A new technique was established to identify eight organophosphate esters (OPEs in this work. It utilised dispersive liquid-liquid microextraction in combination with ultrahigh performance liquid chromatography/tandem mass spectrometry. The type and volume of extraction solvents, dispersion agent, and amount of NaCl were optimized. The target analytes were detected in the range of 1.0–200 µg/L with correlation coefficients ranging from 0.9982 to 0.9998, and the detection limits of the analytes were ranged from 0.02 to 0.07 µg/L (S/N=3. The feasibility of this method was demonstrated by identifying OPEs in aqueous samples that exhibited spiked recoveries, which ranged between 48.7% and 58.3% for triethyl phosphate (TEP as well as between 85.9% and 113% for the other OPEs. The precision was ranged from 3.2% to 9.3% (n=6, and the interprecision was ranged from 2.6% to 12.3% (n=5. Only 2 of the 12 selected samples were tested to be positive for OPEs, and the total concentrations of OPEs in them were 1.1 and 1.6 µg/L, respectively. This method was confirmed to be simple, fast, and accurate for identifying OPEs in aqueous samples.

  17. Separation and determination of copper in bottled water samples by combination of dispersive liquid--liquid microextraction and microsample introduction flame atomic absorption spectrometry.

    Science.gov (United States)

    Citak, Demirhan; Tuzen, Mustafa

    2013-01-01

    A new and simple method for the determination of trace amounts of Cu(II) was developed by combination of dispersive liquid-liquid microextraction (DLLME) preconcentration and microsample introduction flame atomic absorption spectrometry. In this method, ethanol and chloroform were chosen as disperser and extraction solvents, respectively, and 1-nitroso-2-naphthol was used as the complexing agent. The factors affecting the extraction efficiency and determination of Cu(II), including extraction and disperser solvent nature and volume, concentration of the complexing agent, pH of the solution, extraction time, and matrix ions, were investigated. Under optimal conditions, the LOD for Cu(II) was 0.95 microg/L with a preconcentration factor of 70. The RSD was 1.9%. The accuracy of the developed DLLME method was verified by determination of Cu(II) in a certified reference material (NRCC-SLRS-4 river water). The relative error was -3.31%. The developed preconcentration procedure was successfully applied to the analysis of bottled drinking water samples.

  18. Solid phase microextraction of diclofenac using molecularly imprinted polymer sorbent in hollow fiber combined with fiber optic-linear array spectrophotometry.

    Science.gov (United States)

    Pebdani, Arezou Amiri; Shabani, Ali Mohammad Haji; Dadfarnia, Shayessteh; Khodadoust, Saeid

    2015-08-05

    A simple solid phase microextraction method based on molecularly imprinted polymer sorbent in the hollow fiber (MIP-HF-SPME) combined with fiber optic-linear array spectrophotometer has been applied for the extraction and determination of diclofenac in environmental and biological samples. The effects of different parameters such as pH, times of extraction, type and volume of the organic solvent, stirring rate and donor phase volume on the extraction efficiency of the diclofenac were investigated and optimized. Under the optimal conditions, the calibration graph was linear (r(2)=0.998) in the range of 3.0-85.0 μg L(-1) with a detection limit of 0.7 μg L(-1) for preconcentration of 25.0 mL of the sample and the relative standard deviation (n=6) less than 5%. This method was applied successfully for the extraction and determination of diclofenac in different matrices (water, urine and plasma) and accuracy was examined through the recovery experiments. Copyright © 2015 Elsevier B.V. All rights reserved.

  19. Solid-phase extraction combined with dispersive liquid-liquid microextraction for the determination of pyrethroid pesticides in wheat and maize samples.

    Science.gov (United States)

    Zhu, Xiaodan; Jia, Chunhong; Zheng, Zuntao; Feng, Xiaoyuan; He, Yue; Zhao, Ercheng

    2016-12-01

    A rapid, selective and sensitive sample preparation method based on solid-phase extraction combined with the dispersive liquid-liquid microextration was developed for the determination of pyrethroid pesticides in wheat and maize samples. Initially, the samples were extracted with acetonitrile and water solution followed phase separation with the salt addition. The following sample preparation involves a solid-phase extraction and dispersive liquid-liquid microextraction step, which effectively provide cleanup and enrichment effects. The main experimental factors affecting the performance both of solid-phase extraction and dispersive liquid-liquid microextration were investigated. The validation results indicated the suitability of the proposed method for routine analyze of pyrethroid pesticides in wheat and maize samples. The fortified recoveries at three levels ranged between 76.4 and 109.8% with relative standard deviations of less than 10.7%. The limit of quantification of the proposed method was below 0.0125 mg/kg for the pyrethoroid pesticides. The proposed method was successfully used for the rapid determination of pyrethroid residues in real wheat and maize samples from crop field in Beijing, China. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Sensitive Detection of Organophosphorus Pesticides in Medicinal Plants Using Ultrasound-Assisted Dispersive Liquid-Liquid Microextraction Combined with Sweeping Micellar Electrokinetic Chromatography.

    Science.gov (United States)

    Wei, Jin-Chao; Hu, Ji; Cao, Ji-Liang; Wan, Jian-Bo; He, Cheng-Wei; Hu, Yuan-Jia; Hu, Hao; Li, Peng

    2016-02-03

    A simple, rapid, and sensitive method using ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) combined with sweeping micellar electrokinetic chromatography (sweeping-MEKC) has been developed for the determination of nine organophosphorus pesticides (chlorfenvinphos, parathion, quinalphos, fenitrothion, azinphos-ethyl, parathion-methyl, fensulfothion, methidathion, and paraoxon). The important parameters that affect the UA-DLLME and sweeping efficiency were investigated. Under the optimized conditions, the proposed method provided 779.0-6203.5-fold enrichment of the nine pesticides compared to the normal MEKC method. The limits of detection ranged from 0.002 to 0.008 mg kg(-1). The relative standard deviations of the peak area ranged from 1.2 to 6.5%, indicating the good repeatability of the method. Finally, the developed UA-DLLME-sweeping-MEKC method has been successfully applied to the analysis of the investigated pesticides in several medicinal plants, including Lycium chinense, Dioscorea opposite, Codonopsis pilosula, and Panax ginseng, indicating that this method is suitable for the determination of trace pesticide residues in real samples with complex matrices.

  1. Study of the mechanism of acetonitrile stacking and its application for directly combining liquid-phase microextraction with micellar electrokinetic chromatography.

    Science.gov (United States)

    Sun, Jingru; Feng, Jing; Shi, Ludi; Liu, Laping; He, Hui; Fan, Yingying; Hu, Shibin; Liu, Shuhui

    2016-08-26

    Acetonitrile stacking is an online concentration method that is distinctive due to its inclusion of a high proportion of organic solvent in sample matrices. We previously designed a universal methodology for the combination of liquid-phase microextraction (LPME) and capillary electrophoresis (CE) using acetonitrile stacking and micellar electrokinetic chromatography (MEKC) mode, thereby achieving large-volume injection of the diluted LPME extractant and the online concentration. In this report, the methodology was extended to the analysis of highly substituted hydrophobic chlorophenols in wines using diethyl carbonate as the extractant. Additionally, the mechanism of acetonitrile stacking was studied. The results indicated that the combination of LPME and MEKC exhibited good analytical performance: with ∼40-fold concentration by LPME, a 20-cm (33% of the total length) sample plug injection of an eight-fold dilution of diethyl carbonate with the organic solvent-saline solution produced enrichments higher by a factor of 260-791. Limits of qualification ranged from 5.5 to 16.0ng/mL. Acceptable reproducibilities of lower than 1.8% for migration time and 8.6% for peak areas were obtained. A dual stacking mechanism of acetonitrile stacking was revealed, involving transient isotachophoresis plus pH-junction stacking. The latter was associated with a pH shift induced by the presence of acetonitrile. The pseudo-stationary phase (Brij-35) played an important role in reducing the CE running time by weakening the isotachophoretic migration of the analyte ions following Cl(-) ions. The combination of acetonitrile stacking and nonionic micelle-based MEKC appears to be a perfect match for introducing water-immiscible LPME extractants into an aqueous CE system and can thus significantly expand the application of LPME-CE in green analytical chemistry. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. Combined Excimer Laser Photoablation and Amniotic Membrane Overlay for Relief of Symptomatic Discomfort in Gelatinous Drop-like Corneal Dystrophy.

    Science.gov (United States)

    Alex, Anne F; Eter, Nicole; Uhlig, Constantin E

    2015-10-01

    To describe the efficacy of combined excimer laser photoablation and amniotic overlay membrane in the relief of symptomatic discomfort in a 17-year-old patient who had gelatinous drop-like corneal dystrophy. The best-corrected visual acuity (BCVA) was measured with Snellen letters. Slit-lamp examination of the ocular surface and anterior chamber was performed at baseline. Results were photodocumented. Excimer laser photoablation was performed and subsequently 2 amniotic membranes were transconjunctivally fixated with 10.0 nylon sutures. Investigations and documentation were performed at baseline, every 2 months in the first year, and then every 6 months. The duration of follow-up was 22 months. At baseline, the BCVA was 20/70 in the right eye and 20/200 in the left eye. The patient reported distinct photophobia. Slit-lamp examination was difficult because of blepharospasm. Although gelatinous drops developed again and the BCVA decreased to 2/200, the patient reported significant relief after both microsurgical treatments and remained comfortable at 20 and 22 months. Excimer laser photocoagulation combined with amniotic membrane overlay does not stop the development of gelatinous drop-like corneal dystrophy but may improve subjective comfort. Such treatment does not hinder subsequent lamellar or penetrating grafts and is helpful in providing the necessary time for preparation of matched keratoplasties.

  3. Liquid-phase microextraction and fibre-optics-based cuvetteless CCD-array micro-spectrophotometry for trace analysis

    International Nuclear Information System (INIS)

    Sharma, Nisha; Pillai, Aradhana K.K.V.; Pathak, Neeraj; Jain, Archana; Verma, Krishna K.

    2009-01-01

    Liquid-phase microextraction (LPME) has been investigated for trace analysis in the present work in conjunction with fibre-optic-based micro-spectrophotometry which accommodates sample volume of 1 μL placed between the two ends of optical fibres. Methods have been evolved for the determination of (i) 1-100 μM and 0.5-20 μM of thiols by single drop microextraction (SDME) and LPME in 25 μL of the organic solvent, respectively, involving their reaction with the Ellman reagent and ion pair microextraction of thiolate ion formed; (ii) 70 μg to 7 mg L -1 of chlorine/chlorine dioxide by headspace in-drop reaction with alternative reagents, viz., mixed phenylhydrazine-4-sulphonic acid and N-(1-naphthyl)ethylenediamine dihydrochloride, o-dianisidine, o-tolidine, and N,N-diethyl-p-phenylenediamine; (iii) 0.2-4 mg L -1 of ammonia by reaction with 2,4-dinitro-1-fluorobenzene to give 2,4-dinitroaniline which was diazotized and coupled with 1-naphthylamine, the resulting dye was subjected to preconcentration by solid-phase extraction and LPME; and (iv) 25-750 μg L -1 of iodide/total iodine by oxidation of iodide by 2-iodosobenzoate, microextraction of iodine in organic solvent, and re-extraction into aqueous starch-iodide reagent drop held in the organic phase. LPME using 25-30 μL of organic solvent was found to produce more sensitive results than SDME. The cuvetteless spectrophotometry as used in combination with sample handling techniques produced limits of detection of analytes which were better than obtained by previously reported spectrophotometry.

  4. Simultaneous quantification of amphetamines, caffeine and ketamine in urine by hollow fiber liquid phase microextraction combined with gas chromatography-flame ionization detector.

    Science.gov (United States)

    Xiong, Jun; Chen, Jie; He, Man; Hu, Bin

    2010-08-15

    A method of hollow fiber (HF) liquid phase microextraction (LPME) combined with gas chromatography (GC)-flame ionization detection (FID) was developed for the simultaneous quantification of trace amphetamine (AP), methamphetamine (MA), methylenedioxyamphetamine (MDA), methylenedioxymethamphetamine (MDMA), caffeine and ketamine (KT) in drug abuser urine samples. The factors affecting on the extraction of six target analytes by HF-LPME were investigated and optimized, and the subsequent analytical performance evaluation and real sample analysis were performed by the extraction of six target analytes in sample solution containing 30% NaCl (pH 12.5) for 20 min with extraction temperature of 30 degrees C and stirring rate of 1000 rpm. Under such optimal conditions, the limits of detection (LODs, S/N=3) for the six target analytes were ranged from 8 microg/L (AP, KT) to 82 microg/L (MDA), with the enrichment factors (EFs) of 5-227 folds, and the relative standard deviations (RSDs, n=7) were in the range of 6.9-14.1%. The correlation coefficients of the calibration for the six target analytes over the dynamic linear range were higher than 0.9958. The application feasibility of HF-LPME-GC-FID in illegal drug monitoring was demonstrated by analyzing drug abuser urine samples, and the recoveries of target drugs for the spiked sample ranging from 75.2% to 119.3% indicated an excellent anti-interference capability of the developed method. The proposed method is simple, effective, sensitive and low-cost, and provides a much more accurate and sensitive detection platform over the conventional analytical techniques (such as immunological assay) for drug abuse analysis. Copyright 2010 Elsevier B.V. All rights reserved.

  5. Hollow fibre-based liquid-phase microextraction technique combined with gas chromatography-mass spectrometry for the determination of pyrethroid insecticides in water samples.

    Science.gov (United States)

    San Román, I; Alonso, M L; Bartolomé, L; Alonso, R M

    2012-10-15

    A simple, easy-to-use, efficient and environmentally friendly method has been developed for the simultaneous analysis of nine pirethroid pesticides in water samples by the combination of hollow fibre-based liquid-phase microextraction (HF-LPME) and gas chromatography-mass spectrometry (GC/MS). For the developed method, nine pirethroid pesticides (esbiothrin, prallethrin, bifenthrin, tetramethrin, phenothrin, permethrin, cyfluthrin, cypermethrin and deltamethrin) were concentrated and well separated under optimal conditions. Several factors that influence the efficiency of HF-LPME were investigated and optimized by means of experimental design. The proposed method has good linearity in the concentration range of 10-400 μg L(-1) with correlation coefficients between 0.995 and 0.999. Overall enrichment factors for the optimized method ranged from 139 to 255 times except for cypermethrin and deltamethrin which ranged from 35 to 128. Detection and quantitation limits of the chromatographic method were in the range of 0.002-0.012 μg L(-1) and 0.003-0.026 μg L(-1) respectively, with RSD values between 4.2% and 18.4%. The recoveries varied in the range of 69.4%-122.7% except for cypermethrin and deltamethrin (17.5%-64.1%) with relative standard deviations between 1.0% and 24.0% for intra and inter-day experiments at different concentrations (0.1 μg L(-1), 0.5 μg L(-1), 1 μg L(-1)). The HF-LPME method optimized was applied to the analysis of three spiked real water samples with good results. Copyright © 2012 Elsevier B.V. All rights reserved.

  6. A combined coalescence gene-dropping tool for evaluating genomic selection in complex scenarios (ms2gs).

    Science.gov (United States)

    Pérez-Enciso, M; Legarra, A

    2016-04-01

    We present ms2gs, a combined coalescence - gene dropping (i.e. backward-forward) simulator for complex traits. It therefore aims at combining the advantages of both approaches. It is primarily conceived for very short term, recent scenarios such as those that are of interest in animal and plant breeding. It is very flexible in terms of defining QTL architecture and SNP ascertainment bias, and it allows for easy modelling of alternative markers such as RADs. It can use real sequence or chip data or generate molecular polymorphisms via the coalescence. It can generate QTL conditional on extant molecular information, such as low-density genotyping. It models (simplistically) sequence, imputation or genotyping errors. It requires as input both genotypic data in plink or ms formats, and a pedigree that is used to perform the gene dropping. By default, it compares accuracy for BLUP, SNP ascertained data, sequence, and causal SNPs. It employs VanRaden's linear (GBLUP) and nonlinear method for incorporating molecular information. To illustrate the program, we present a small application in a half-sib population and a multiparental (MAGIC) cross. The program, manual and examples are available at https://github.com/mperezenciso/ms2gs. © 2016 Blackwell Verlag GmbH.

  7. Integral linear momentum balance in combining flows for calculating the pressure drop coefficients

    International Nuclear Information System (INIS)

    Bollmann, A.

    1983-01-01

    Equations for calculating the loss coefficient in combining flows in tee functions are obtained by an integral linear momentum balance. It is a practice, when solving this type of problem, to neglect the pressure difference in the upstream location as well as the wall-fluid interaction in the lateral branch of the junction. In this work it is demonstrated the influence of the above parameters on the loss coefficient based on experimental values and by apropriate algebraic manipulation of the loss coefficient values published by previous investigators. (Author) [pt

  8. Silica- and germania-based dual-ligand sol-gel organic-inorganic hybrid sorbents combining superhydrophobicity and π-π interaction. The role of inorganic substrate in sol-gel capillary microextraction.

    Science.gov (United States)

    Seyyal, Emre; Malik, Abdul

    2017-04-29

    Principles of sol-gel chemistry were utilized to create silica- and germania-based dual-ligand surface-bonded sol-gel coatings providing enhanced performance in capillary microextraction (CME) through a combination of ligand superhydrophobicity and π-π interaction. These organic-inorganic hybrid coatings were prepared using sol-gel precursors with bonded perfluorododecyl (PF-C 12 ) and phenethyl (PhE) ligands. Here, the ability of the PF-C 12 ligand to provide enhanced hydrophobic interaction was advantageously combined with π-π interaction capability of the PhE moiety to attain the desired sorbent performance in CME. The effect of the inorganic sorbent component on microextraction performance of was explored by comparing microextraction characteristics of silica- and germania-based sol-gel sorbents. The germania-based dual-ligand sol-gel sorbent demonstrated superior CME performance compared to its silica-based counterpart. Thermogravimetric analysis (TGA) of the created silica- and germania-based dual-ligand sol-gel sorbents suggested higher carbon loading on the germania-based sorbent. This might be indicative of more effective condensation of the organic ligand-bearing sol-gel-active chemical species to the germania-based sol-gel network (than to its silica-based counterpart) evolving in the sol solution. The type and concentration of the organic ligands were varied in the sol-gel sorbents to fine-tune extraction selectivity toward different classes of analytes. Specific extraction (SE) values were used for an objective comparison of the prepared sol-gel CME sorbents. The sorbents with higher content of PF-C 12 showed remarkable affinity for aliphatic hydrocarbons. Compared to their single-ligand sol-gel counterparts, the dual-ligand sol-gel coatings demonstrated significantly superior CME performance in the extraction of alkylbenzenes, providing up to ∼65.0% higher SE values. The prepared sol-gel CME coatings provided low ng L -1 limit of detections (LOD

  9. Enrichment of copper as 1-(2-pyridylazo)-2-naphthol complex by the combination of dispersive liquid-liquid microextraction/flame atomic absorption spectrometry.

    Science.gov (United States)

    Kandhro, Ghulam A; Soylak, Mustafa; Kazi, Tasneem Gul; Yilmaz, Erkan

    2014-01-01

    A rapid, simple, selective, economical, and sensitive dispersive liquid-liquid microextraction methodology has been established for the preconcentration of copper (Cu) at trace levels. The Cu(II) was complexed with 1-(2-pyridylazo)-2-naphthol; ethanol and carbon tetrachloride were used as disperser and extraction solvents, respectively. To obtain quantitative recovery of Cu(II), the effects of parameters influencing its extraction efficiency and subsequent determinations, i.e., pH, amount of complexing reagent, extraction time, and type and volume of disperser and extraction solvents, were examined. LOD and LOQ were 0.06 and 0.20 microg/L, respectively. The enrichment factor of the proposed method was 60, and the RSD <5%. TMDA 51.3 and TMDA 70 fortified water certified reference materials were analyzed for validation of the procedure. The developed microextraction procedure has been used for the preconcentration of Cu(II) in water samples with acceptable results.

  10. Simultaneous derivatization and ultrasound-assisted dispersive liquid-liquid microextraction of chloropropanols in soy milk and other aqueous matrices combined with gas-chromatography-mass spectrometry.

    Science.gov (United States)

    Carro, A M; González, P; Lorenzo, R A

    2013-12-06

    A novel approach involving ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) and derivatization combined with gas chromatography-mass spectrometry was developed for the determination of chloropropanols in water and beverages. UA-DLLME was optimized as less solvent-consuming and cost-effective extraction method for water, fruit juice, milk and soy milk samples. The effect of parameters such as the type and volume of extraction solvent, the type and volume of dispersive solvent, amount of derivatization agent, temperature, pH of sample and ionic strength was investigated and optimized for each specimen, using experimental designs. By adding acetonitrile as dispersive solvent, N-heptafluorobutyrylimizadole (HFBI) as derivatization agent and chloroform as extraction solvent, the extraction-derivatization and preconcentration were simultaneously performed. The analytical concentration range was investigated in detail for each analyte in the different samples, obtaining linearity with R(2) ranging between 0.9990 and 0.9999. The method detection limits were in the range of 0.2-1.8μgL(-1) (water), 0.5-15μgL(-1) (fruit juices) and 0.9-3.6μgkg(-1) (milk) and 0.1-1.0μgkg(-1) (soy milk). The method was applied to the analysis of a variety of specimens, with recoveries of 98-101% from water, 97-102% from juices, 99-103% from milk and 97-105% from soy beverage. The relative standard deviation (precision, n=6) varied between 1.3 and 4.9%RSD in water, 2.3 and 5.8%RSD in juices, 1.0 and 5.7%RSD in milk and 3.9 and 9.3%RSD in soy milk. The proposed method was applied to analysis of twenty-eight samples. 1,3-Dichloro-2-propanol was found in an influent water sample from urban wastewater treatment plant (WWTP) (2.1±0.04mgL(-1)) but no chloropropanols were found in the corresponding effluent water sample. This result suggests that the purification system used in the WWTP has been effective for this compound. Moreover, the results revealed the presence of 3

  11. In-situ ionic liquid dispersive liquid-liquid microextraction using a new anion-exchange reagent combined Fe3O4magnetic nanoparticles for determination of pyrethroid pesticides in water samples.

    Science.gov (United States)

    Fan, Chen; Liang, You; Dong, Hongqiang; Ding, Guanglong; Zhang, Wenbing; Tang, Gang; Yang, Jiale; Kong, Dandan; Wang, Deng; Cao, Yongsong

    2017-07-04

    In this work, in-situ ionic liquid dispersive liquid-liquid microextraction combined ultrasmall Fe 3 O 4 magnetic nanoparticles was developed as a kind of pretreatment method to detect pyrethroid pesticides in water samples. New anion-exchange reagents including Na[DDTC] and Na[N(CN) 2 ] were optimized for in-situ extraction pyrethroids, which showed enhanced microextraction performance. Pyrethroids were enriched by hydrophilic ionic liquid [P 4448 ][Br] (aqueous solution, 200 μL, 0.2 mmol mL -1 ) reaction in-situ with anion-exchange reagent Na[N(CN) 2 ] (aqueous solution, 300 μL, 0.2 mmol mL -1 ) forming hydrophobic ionic liquid as extraction agent in water sample (10 mL). Ultrasmall superparamagnetic iron oxide nanoparticles (30 mg) were used to collect the mixture of ionic liquid and pyrethroids followed by elution with acetonitrile. The extraction of ionic liquid strategies was unique and efficiently fulfilled with high enrichment factors (176-213) and good recoveries (80.20-117.31%). The method was successively applied to the determination of pyrethroid pesticides in different kinds of water samples with the limits of detection ranged from 0.16 to 0.21 μg L -1 . The proposed method is actually nanometer-level microextraction (average size 80 nm) with the advantages of simplicity, rapidity, and sensitivity. Copyright © 2017 Elsevier B.V. All rights reserved.

  12. Development of a New Microextraction Fiber Combined to On-Line Sample Stacking Capillary Electrophoresis UV Detection for Acidic Drugs Determination in Real Water Samples

    Directory of Open Access Journals (Sweden)

    Maria Espina-Benitez

    2017-07-01

    Full Text Available A new analytical method coupling a (off-line solid-phase microextraction with an on-line capillary electrophoresis (CE sample enrichment technique was developed for the analysis of ketoprofen, naproxen and clofibric acid from water samples, which are known as contaminants of emerging concern in aquatic environments. New solid-phase microextraction fibers based on physical coupling of chromatographic supports onto epoxy glue coated needle were studied for the off-line preconcentration of these micropollutants. Identification and quantification of such acidic drugs were done by capillary zone electrophoresis (CZE using ultraviolet diode array detection (DAD. Further enhancement of concentration sensitivity detection was achieved by on-line CE “acetonitrile stacking” preconcentration technique. Among the eight chromatographic supports investigated, Porapak Q sorbent showed higher extraction and preconcentration capacities. The screening of parameters that influence the microextraction process was carried out using a two-level fractional factorial. Optimization of the most relevant parameters was then done through a surface response three-factor Box-Behnken design. The limits of detection and limits of quantification for the three drugs ranged between 0.96 and 1.27 µg∙L−1 and 2.91 and 3.86 µg∙L−1, respectively. Recovery yields of approximately 95 to 104% were measured. The developed method is simple, precise, accurate, and allows quantification of residues of these micropollutants in Genil River water samples using inexpensive fibers.

  13. Ultrapreconcentration and determination of organophosphorus pesticides in water by solid-phase extraction combined with dispersive liquid-liquid microextraction and high-performance liquid chromatography.

    Science.gov (United States)

    Chen, Junhua; Zhou, Guangming; Deng, Yongli; Cheng, Hongmei; Shen, Jie; Gao, Yi; Peng, Guilong

    2016-01-01

    Solid-phase extraction coupled with dispersive liquid-liquid microextraction was developed as an ultra-preconcentration method for the determination of four organophosphorus pesticides (isocarbophos, parathion-methyl, triazophos and fenitrothion) in water samples. The analytes considered in this study were rapidly extracted and concentrated from large volumes of aqueous solutions (100 mL) by solid-phase extraction coupled with dispersive liquid-liquid microextraction and then analyzed using high performance liquid chromatography. Experimental variables including type and volume of elution solvent, volume and flow rate of sample solution, salt concentration, type and volume of extraction solvent and sample solution pH were investigated for the solid-phase extraction coupled with dispersive liquid-liquid microextraction with these analytes, and the best results were obtained using methanol as eluent and ethylene chloride as extraction solvent. Under the optimal conditions, an exhaustive extraction for four analytes (recoveries >86.9%) and high enrichment factors were attained. The limits of detection were between 0.021 and 0.15 μg/L. The relative standard deviations for 0.5 μg/L of the pesticides in water were in the range of 1.9-6.8% (n = 5). The proposed strategy offered the advantages of simple operation, high enrichment factor and sensitivity and was successfully applied to the determination of four organophosphorus pesticides in water samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Microextraction sample preparation techniques in biomedical analysis.

    Science.gov (United States)

    Szultka, Malgorzata; Pomastowski, Pawel; Railean-Plugaru, Viorica; Buszewski, Boguslaw

    2014-11-01

    Biologically active compounds are found in biological samples at relatively low concentration levels. The sample preparation of target compounds from biological, pharmaceutical, environmental, and food matrices is one of the most time-consuming steps in the analytical procedure. The microextraction techniques are dominant. Metabolomic studies also require application of proper analytical technique for the determination of endogenic metabolites present in biological matrix on trace concentration levels. Due to the reproducibility of data, precision, relatively low cost of the appropriate analysis, simplicity of the determination, and the possibility of direct combination of those techniques with other methods (combination types on-line and off-line), they have become the most widespread in routine determinations. Additionally, sample pretreatment procedures have to be more selective, cheap, quick, and environmentally friendly. This review summarizes the current achievements and applications of microextraction techniques. The main aim is to deal with the utilization of different types of sorbents for microextraction and emphasize the use of new synthesized sorbents as well as to bring together studies concerning the systematic approach to method development. This review is dedicated to the description of microextraction techniques and their application in biomedical analysis. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Rapid and sensitive determination of phytosterols in functional foods and medicinal herbs by using UHPLC-MS/MS with microwave-assisted derivatization combined with dual ultrasound-assisted dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Sun, Jing; Zhao, Xian-En; Dang, Jun; Sun, Xiaoyan; Zheng, Longfang; You, Jinmao; Wang, Xiao

    2017-02-01

    In this work, a hyphenated technique of dual ultrasound-assisted dispersive liquid-liquid microextraction combined with microwave-assisted derivatization followed by ultra high performance liquid chromatography tandem mass spectrometry has been developed for the determination of phytosterols in functional foods and medicinal herbs. Multiple reaction monitoring mode was used for the tandem mass spectrometry detection. A mass spectrometry sensitive reagent, 4'-carboxy-substituted rosamine, has been used as the derivatization reagent for five phytosterols, and internal standard diosgenin was used for the first time. Parameters for the dual microextraction, microwave-assisted derivatization, and ultra high performance liquid chromatography tandem mass spectrometry were all optimized in detail. Satisfactory linearity, recovery, repeatability, accuracy and precision, absence of matrix effect, extremely low limits of detection (0.005-0.015 ng/mL) and limits of quantification (0.030-0.10 ng/mL) were achieved. The proposed method was compared with previously reported methods. It showed better sensitivity, selectivity, and accuracy. The matrix effect was also significantly reduced. The proposed method was successfully applied to the determination of five phytosterols in vegetable oil (sunflower oil, olive oil, corn oil, peanut oil), milk and orange juice (soymilk, peanut milk, orange juice), and medicinal herbs (Ginseng, Ganoderma lucidum, Cordyceps, Polygonum multiflorum) for the quality control of functional foods and medicinal herbs. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Non-targeted volatile profiles for the classification of the botanical origin of Chinese honey by solid-phase microextraction and gas chromatography-mass spectrometry combined with chemometrics.

    Science.gov (United States)

    Chen, Hui; Jin, Linghe; Fan, Chunlin; Wang, Wenwen

    2017-11-01

    A potential method for the discrimination and prediction of honey samples of various botanical origins was developed based on the non-targeted volatile profiles obtained by solid-phase microextraction with gas chromatography and mass spectrometry combined with chemometrics. The blind analysis of non-targeted volatile profiles was carried out using solid-phase microextraction with gas chromatography and mass spectrometry for 87 authentic honey samples from four botanical origins (acacia, linden, vitex, and rape). The number of variables was reduced from 2734 to 70 by using a series of filters. Based on the optimized 70 variables, 79.12% of the variance was explained by the first four principal components. Partial least squares discriminant analysis, naïve Bayes analysis, and back-propagation artificial neural network were used to develop the classification and prediction models. The 100% accuracy revealed a perfect classification of the botanical origins. In addition, the reliability and practicability of the models were validated by an independent set of additional 20 authentic honey samples. All 20 samples were accurately classified. The confidence measures indicated that the performance of the naïve Bayes model was better than the other two models. Finally, the characteristic volatile compounds of linden honey were tentatively identified. The proposed method is reliable and accurate for the classification of honey of various botanical origins. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Combination of solid phase extraction and dispersive liquid-liquid microextraction for separation/preconcentration of ultra trace amounts of uranium prior to its fiber optic-linear array spectrophotometry determination.

    Science.gov (United States)

    Dadfarnia, Shayessteh; Shabani, Ali Mohammad Haji; Shakerian, Farid; Shiralian Esfahani, Golnaz

    2013-12-15

    A simple and sensitive method for the separation and preconcentration of the ultra trace amounts of uranium and its determination by spectrophotometry was developed. The method is based on the combination of solid phase extraction and dispersive liquid-liquid microextraction. Thus, by passing the sample through the basic alumina column, the uranyl ion and some cations are separated from the sample matrix. The retained uranyl ion along with the cations are eluted with 5 mL of nitric acid (2 mol L(-1)) and after neutralization of the eluent, the extracted uranyl ion is converted to its anionic benzoate complex and is separated from other cations by extraction of its ion pair with malachite green into small volume of chloroform using dispersive liquid-liquid microextraction. The amount of uranium is then determined by the absorption measurement of the extracted ion pair at 621 nm using flow injection spectrophotometry. Under the optimum conditions, with 500 mL of the sample, a preconcentration factor of 1980, a detection limit of 40 ng L(-1), and a relative standard deviation of 4.1% (n=6) at 400 ng L(-1) were obtained. The method was successfully applied to the determination of uranium in mineral water, river water, well water, spring water and sea water samples. Copyright © 2013 Elsevier B.V. All rights reserved.

  18. Trace determination of five triazole fungicide residues in traditional Chinese medicine samples by dispersive solid-phase extraction combined with ultrasound-assisted dispersive liquid-liquid microextraction and UHPLC-MS/MS.

    Science.gov (United States)

    Ma, Shuping; Yuan, Xucan; Zhao, Pengfei; Sun, Hong; Ye, Xiu; Liang, Ning; Zhao, Longshan

    2017-08-01

    A novel and reliable method for determination of five triazole fungicide residues (triadimenol, tebuconazole, diniconazole, flutriafol, and hexaconazol) in traditional Chinese medicine samples was developed using dispersive solid-phase extraction combined with ultrasound-assisted dispersive liquid-liquid microextraction before ultra-high performance liquid chromatography with tandem mass spectrometry. The clean up of the extract was conducted using dispersive solid-phase extraction by directly adding sorbents into the extraction solution, followed by shaking and centrifugation. After that, a mixture of 400 μL trichloromethane (extraction solvent) and 0.5 mL of the above supernatant was injected rapidly into water for the dispersive liquid-liquid microextraction procedure. The factors affecting the extraction efficiency were optimized. Under the optimum conditions, the calibration curves showed good linearity in the range of 2.0-400 (tebuconazole, diniconazole, and hexaconazole) and 4.0-800 ng/g (triadimenol and flutriafol) with the regression coefficients higher than 0.9958. The limit of detection and limit of quantification for the present method were 0.5-1.1 and 1.8-4.0 ng/g, respectively. The recoveries of the target analytes ranged from 80.2 to 103.2%. The proposed method has been successfully applied to the analysis of five triazole fungicides in traditional Chinese medicine samples, and satisfactory results were obtained. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. A novel extraction technique based on carbon nanotubes reinforced hollow fiber solid/liquid microextraction for the measurement of piroxicam and diclofenac combined with high performance liquid chromatography.

    Science.gov (United States)

    Song, Xin-Yue; Shi, Yan-Ping; Chen, Juan

    2012-10-15

    A novel design of carbon nanotubes reinforced hollow fiber solid/liquid phase microextraction (CNTs-HF-SLPME) was developed to determine piroxicam and diclofenac in different real water samples. Functionalized multi-walled carbon nanotubes (MWCNTs) were held in the pores of hollow fiber with sol-gel technology. The pores and lumen of carbon nanotubes reinforced hollow fiber were subsequently filled with a μL volume of organic solvent (1-octanol), and then the whole assembly was used for the extraction of the target analytes in direct immersion sampling mode. The target analytes were extracted from the sample by two extractants, one of which is organic solvent placed inside the pores and lumen of hollow fiber and the other one is CNTs held in the pores of hollow fiber. After extraction, the analytes were desorbed in acetonitrile and analyzed using high performance liquid chromatography. This novel extraction mode showed more excellent extraction performance in comparison with conventional hollow fiber liquid microextraction (without adding CNTs) and carbon nanotubes reinforced hollow fiber solid microextraction (CNTs held in the pores of hollow fiber, but no organic solvents placed inside the lumen of hollow fiber) under the respective optimum conditions. This method provided 47- and 184-fold enrichment factors for piroxicam and diclofenac, respectively, good inter-fiber repeatability and batch-to-batch reproducibility. Linearity was observed in the range of 20-960 μg L(-1) for piroxicam, and 10-2560 μg L(-1) for diclofenac, with correlation coefficients of 0.9985 and 0.9989, respectively. The limits of detection were 4.58 μg L(-1) for piroxicam and 0.40 μg L(-1) for diclofenac. Copyright © 2012 Elsevier B.V. All rights reserved.

  20. Non-conventional solvents in liquid phase microextraction and aqueous biphasic systems.

    Science.gov (United States)

    An, Jiwoo; Trujillo-Rodríguez, María J; Pino, Verónica; Anderson, Jared L

    2017-06-02

    The development of rapid, convenient, and high throughput sample preparation approaches such as liquid phase microextraction techniques have been continuously developed over the last decade. More recently, significant attention has been given to the replacement of conventional organic solvents used in liquid phase microextraction techniques in order to reduce toxic waste and to improve selectivity and/or extraction efficiency. With these objectives, non-conventional solvents have been explored in liquid phase microextraction and aqueous biphasic systems. The utilized non-conventional solvents include ionic liquids, magnetic ionic liquids, and deep eutectic solvents. They have been widely used as extraction solvents or additives in various liquid phase microextraction modes including dispersive liquid-liquid microextraction, single-drop microextraction, hollow fiber-liquid phase microextraction, as well as in aqueous biphasic systems. This review provides an overview into the use of non-conventional solvents in these microextraction techniques in the past 5 years (2012-2016). Analytical applications of the techniques are also discussed. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. Green aspects, developments and perspectives of liquid phase microextraction techniques.

    Science.gov (United States)

    Spietelun, Agata; Marcinkowski, Łukasz; de la Guardia, Miguel; Namieśnik, Jacek

    2014-02-01

    Determination of analytes at trace levels in complex samples (e.g. biological or contaminated water or soils) are often required for the environmental assessment and monitoring as well as for scientific research in the field of environmental pollution. A limited number of analytical techniques are sensitive enough for the direct determination of trace components in samples and, because of that, a preliminary step of the analyte isolation/enrichment prior to analysis is required in many cases. In this work the newest trends and innovations in liquid phase microextraction, like: single-drop microextraction (SDME), hollow fiber liquid-phase microextraction (HF-LPME), and dispersive liquid-liquid microextraction (DLLME) have been discussed, including their critical evaluation and possible application in analytical practice. The described modifications of extraction techniques deal with system miniaturization and/or automation, the use of ultrasound and physical agitation, and electrochemical methods. Particular attention was given to pro-ecological aspects therefore the possible use of novel, non-toxic extracting agents, inter alia, ionic liquids, coacervates, surfactant solutions and reverse micelles in the liquid phase microextraction techniques has been evaluated in depth. Also, new methodological solutions and the related instruments and devices for the efficient liquid phase micoextraction of analytes, which have found application at the stage of procedure prior to chromatographic determination, are presented. © 2013 Published by Elsevier B.V.

  2. [Gastric dynamics analysis of TEAS combined SNP induced general anesthesia when controlled hypotension dropped to 60% of the MAP baseline].

    Science.gov (United States)

    Zhang, Le-Le; Fang, Jian-Qiao; Shao, Xiao; Lian, Lin-Li; Yu, Xiao-Jing; Dong, Zhen-Hua; Mo, Ya-Di

    2015-01-01

    To observe the effect of gastric dynamics by transcutaneous electrical acupoint stimulation (TEAS) combined general anesthesia when controlled hypotension dropped to 60% of the mean arterial prenssure (MAP) baseline, and to provide experimental evidence for organ protection in clinical controlled hypotension. Eighteen male beagles were randomly divided into three groups, the general anesthesia group (blank), the general anesthesia induced controlled hypotension group (control), and the general anesthesia combined TEAS induced controlled hypotension group (experiment), 6 in each group. Controlled hypotension was performed in the latter two groups with isoflurane inhalation and intravenous injection of sodium nitroprusside (SNP). The mean arterial pressure (MAP) was lowered to 60% of the MAP baseline and kept for 60 min. Controlled hypotension was not performed in Beagles of the control group. For Beagles in the experiment group, TEAS [2/100 Hz, (4 ± 1) mA] was applied to bilateral Hegu (LI4), Quchi (LI11), Zusanli (ST36), and Sanyinjiao (SP6) from stable physiological conditions to the end of maintaining stages. Changes of EGG frequencies and EGG amplitudes were monitored. Serum levels of gastrin (GAS) and motilin (MTL) were also detected at corresponding time points during and after experiment. As for the pressure control effect of TEAS combined general anesthesia in the controlled hypotension, during the process of controlled hypotension (T1-T4), MAP levels of two controlled pressure groups remained relatively stable, and were kept at 60% of the MAP baseline. When the blood pressure dropped to the target low MAP and maintained at 60 min (T1-T4), EGG amplitudes of Beagles in all the three groups showed decreasing tendency. But it was more obviously lower than its basic level in the control group (P control group and the blank group (P control group. During this period, EGG frequencies of the two controlled hypotension groups decreased more than those of the blank

  3. A liquid-phase microextraction method, combining a dual gauge microsyringe with a hollow fiber membrane, for the determination of organochlorine pesticides in aqueous solution by gas chromatography/ion trap mass spectrometry.

    Science.gov (United States)

    Yan, Chih-Hao; Wu, Hui-Fen

    2004-01-01

    A liquid-phase microextraction (LPME) method has been demonstrated for the extraction and determination of organochlorine pesticides (OCPs) in aqueous solution. The method combines a dual gauge microsyringe with a hollow fiber membrane (LPME/DGM-HF) followed by detection by gas chromatography/ion trap mass spectrometry (GC/ITMS). The advantages include speed, low solvent and sample consumption, simplicity and ease of use. The extraction time, solvent selection, salt concentration and sample stirring rate have been investigated in order to optimize extraction efficiency. The viability is evaluated by measuring the linearity and detection limit of the five OCPs in aqueous solution. Detection linearity for the OCPs has been achieved over a range of concentrations between 1 and 500 microg/L (r2 > 0.930), with a detection limit of 0.1 microg/L for each OCP. Copyright 2004 John Wiley & Sons, Ltd.

  4. High performance ceria-bismuth bilayer electrolyte low temperature solid oxide fuel cells (LT-SOFCs) fabricated by combining co-pressing with drop-coating

    KAUST Repository

    Hou, Jie

    2015-03-24

    The Sm0.075Nd0.075Ce0.85O2-δ-Er0.4Bi1.6O3 bilayer structure film, which showed an encouraging performance in LT-SOFCs, was successfully fabricated by a simple low cost technique combining one-step co-pressing with drop-coating.

  5. Applicability of solid-phase microextraction combined with gas chromatography atomic emission detection (GC-MIP AED) for the determination of butyltin compounds in sediment samples

    Energy Technology Data Exchange (ETDEWEB)

    Carpinteiro, J.; Rodriguez, I.; Cela, R. [Universidad de Santiago de Compostela, Departamento de Quimica Analitica, Nutricion y Bromatologia, Instituto de Investigacion y Analisis Alimentario, Santiago de Compostela 15782 (Spain)

    2004-11-01

    The performance of solid-phase microextraction (SPME) applied to the determination of butyltin compounds in sediment samples is systematically evaluated. Matrix effects and influence of blank signals on the detection limits of the method are studied in detail. The interval of linear response is also evaluated in order to assess the applicability of the method to sediments polluted with butyltin compounds over a large range of concentrations. Advantages and drawbacks of including an SPME step, instead of the classic liquid-liquid extraction of the derivatized analytes, in the determination of butyltin compounds in sediment samples are considered in terms of achieved detection limits and experimental effort. Analytes were extracted from the samples by sonication using glacial acetic acid. An aliquot of the centrifuged extract was placed on a vial where compounds were ethylated and concentrated on a PDMS fiber using the headspace mode. Determinations were carried out using GC-MIP AED. (orig.)

  6. Hollow fiber-based liquid phase microextraction combined with high-performance liquid chromatography for extraction and determination of some antidepressant drugs in biological fluids.

    Science.gov (United States)

    Esrafili, Ali; Yamini, Yadollah; Shariati, Shahab

    2007-12-05

    The applicability of hollow fiber-based liquid phase microextraction (HF-LPME) was evaluated for the extraction and preconcentration of three antidepressant drugs (amitriptyline, imipramine and sertraline) prior to their determination by HPLC-UV. The target drugs were extracted from 11.0 mL of aqueous solution with pH 12.0 (source phase) into an organic extracting solvent (n-dodecane) impregnated in the pores of a hollow fiber and finally back extracted into 24 microL of aqueous solution located inside the lumen of the hollow fiber and adjusted to pH 2.1 using 0.1M of H3PO4 (receiving phase). The extraction was performed due to pH gradient between the inside and outside of the hollow fiber membrane. In order to obtain high extraction efficiency, the parameters affecting the HF-LPME including pH of the source and receiving phases, the type of organic phase, ionic strength and volume of the source phase, stirring rate and extraction time were studied and optimized. Under the optimized conditions, enrichment factors up to 300 were achieved and the relative standard deviation (R.S.D.%) of the method was in the range of 2-12%. The calibration curves were obtained in the range of 5-500 microg L(-1) with reasonable linearity (R2>0.998) and the limits of detection (LODs) ranged between 0.5 and 0.7 microg L(-1) (based on S/N=3). Finally, the applicability of the proposed method was evaluated by extraction and determination of the drugs in urine, plasma and tap water samples. The results indicated that hollow fiber microextraction method has excellent clean-up and high-preconcentration factor and can be served as a simple and sensitive method for monitoring of antidepressant drugs in the biological samples.

  7. Solid-phase extraction in combination with dispersive liquid-liquid microextraction and ultra-high performance liquid chromatography-tandem mass spectrometry analysis: the ultra-trace determination of 10 antibiotics in water samples.

    Science.gov (United States)

    Liang, Ning; Huang, Peiting; Hou, Xiaohong; Li, Zhen; Tao, Lei; Zhao, Longshan

    2016-02-01

    A novel method, solid-phase extraction combined with dispersive liquid-liquid microextraction (SPE-DLLME), was developed for ultra-preconcentration of 10 antibiotics in different environmental water samples prior to ultra-high performance liquid chromatography-tandem mass spectrometry detection. The optimized results were obtained as follows: after being adjusted to pH 4.0, the water sample was firstly passed through PEP-2 column at 10 mL min(-1), and then methanol was used to elute the target analytes for the following steps. Dichloromethane was selected as extraction solvent, and methanol/acetonitrile (1:1, v/v) as dispersive solvent. Under optimal conditions, the calibration curves were linear in the range of 1-1000 ng mL(-1) (sulfamethoxazole, cefuroxime axetil), 5-1000 ng mL(-1) (tinidazole), 10-1000 ng mL(-1) (chloramphenicol), 2-1000 ng mL(-1) (levofloxacin oxytetracycline, doxycycline, tetracycline, and ciprofloxacin) and 1-400 ng mL(-1) (sulfadiazine) with a good precision. The LOD and LOQ of the method were at very low levels, below 1.67 and 5.57 ng mL(-1), respectively. The relative recoveries of the target analytes were in the range from 64.16% to 99.80% with relative standard deviations between 0.7 and 8.4%. The matrix effect of this method showed a great decrease compared with solid-phase extraction and a significant value of enrichment factor (EF) compared with dispersive liquid-liquid microextraction. The developed method was successfully applied to the extraction and analysis of antibiotics in different water samples with satisfactory results.

  8. Comparison of micellar extraction combined with ionic liquid based vortex-assisted liquid-liquid microextraction and modified quick, easy, cheap, effective, rugged, and safe method for the determination of difenoconazole in cowpea.

    Science.gov (United States)

    Chen, Xiaochu; Bian, Yanli; Liu, Fengmao; Teng, Peipei; Sun, Pan

    2017-10-06

    Two simple sample pretreatment for the determination of difenoconazole in cowpea was developed including micellar extraction combined with ionic liquid based vortex-assisted liquid-liquid microextraction (ME-IL-VALLME) prior to high performance liquid chromatography (HPLC), and modified quick, easy, cheap, effective, rugged, and safe method (QuEChERS) coupled with HPLC-MS/MS. In ME-IL-VALLME method, the target analyte was extracted by surfactant Tween 20 micellar solution, then the supernatant was diluted with 3mL water to decrease the solubility of micellar solution. Subsequently, the vortex-assisted liquid-liquid microextraction (VALLME) procedure was performed in the diluted extraction solution by using the ionic liquid of 1-hexyl-3-methylimidazolium hexafluorophosphate ([HMIM]PF 6 ) as the extraction solvent and Tween 20 as an emulsifier to enhance the dispersion of the water-immiscible ionic liquid into the aqueous phase. Parameters that affect the extraction have been investigated in both methods Under the optimum conditions, the limits of quantitation were 0.10 and 0.05mgkg -1 , respectively. And good linearity was achieved with the correlation coefficient higher than 0.9941. The relative recoveries ranged from 78.6 to 94.8% and 92.0 to 118.0% with the relative standard deviations (RSD) of 7.9-9.6% and 1.2-3.2%, respectively. Both methods were quick, simple and inexpensive. However, the ME-IL-VALLME method provides higher enrichment factor compared with conventional QuEChERS method. The ME-IL-VALLME method has a strong potential for the determination of difenoconazole in complex vegetable matrices with HPLC. Copyright © 2017 Elsevier B.V. All rights reserved.

  9. Water-contained surfactant-based vortex-assisted microextraction method combined with liquid chromatography for determination of synthetic antioxidants from edible oil.

    Science.gov (United States)

    Amlashi, Nadiya Ekbatani; Hadjmohammadi, Mohammad Reza; Nazari, Seyed Saman Seyed Jafar

    2014-09-26

    For the first time, a novel water-contained surfactant-based vortex-assisted microextraction method (WSVAME) was developed for the extraction of two synthetic antioxidants (t-butyl hydroquinone (TBHQ) and butylated hydroxyanisole (BHA)) from edible oil samples. The novel microextraction method is based on the injection of an aqueous solution of non-ionic surfactant, Brij-35, into the oil sample in a conical bottom glass tube to form a cloudy solution. Vortex mixing was applied to accelerate the dispersion process. After extraction and phase separation by centrifugation, the lower sediment phase was directly analyzed by HPLC. The effects of the four experimental parameters including volume and concentration of extraction solvent (aqueous solution of Brij-35), percentage of acetic acid added to the oil sample and vortex time on the extraction efficiency were studied with a full factorial design. The central composite design and multiple linear regression method were applied for the construction of the best polynomial model based on experimental recoveries. The proposed method showed good linearity within the range of 0.200-200 μg mL(-1), the square of correlation coefficient higher than 0.999 and appropriate limit of detection (0.026 and 0.020 μg mL(-1) for TBHQ and BHA, respectively), while the precision for inner-day was ≤ 3.0 (n=5) and it was ≤ 3.80 (n=5) for inter-day assay. Under the optimal condition (30 μL of 0.10 mol L(-1) Brij-35 solution as extraction solvent and vortex time 1 min), the method was successfully applied for determination of TBHQ and BHA in different commercial edible oil samples. The recoveries in all cases were above 95%, with relative standard deviations below 5%. This approach is considered as a simple, sensitive and environmentally friendly method because of biodegradability of the extraction phase and no use of organic solvent in the extraction procedure. Copyright © 2014 Elsevier B.V. All rights reserved.

  10. A Paper-Based Analytical Device Based on Combination of Thin Film Microextraction and Reflection Scanometry for Sensitive Colorimetric Determination of Ni(II) in Aqueous Matrix.

    Science.gov (United States)

    Allafchian, Ali Reza; Farajmand, Bahman; Koupaei, Amin Javaheri

    2018-02-19

    In this research, the thin film microextraction method was applied for the extraction of Ni(II) ion from aqueous matrixes. Chemically modified cellulosic filter paper with phosphorus was used as a thin film extractor. After extraction, the thin film was treated with a solution of dimethylglyoxime. The colored film was captured by flatbed scanner and the absorbance of the images was extracted by some suitable software. Under the optimum conditions and at the pH 7.0, with the sample volume of 100 mL, the stirring rate of 800 rpm, and the extraction time of 50 min, the calibration curve was obtained in the range of 0.05-5 mg/L Ni(II) (R 2  = 0.989). Limit and relative standard deviation were achieved to be 18 µg/L and less than 6.7%, respectively. Relative recoveries were obtained in the range of 87%-105%. Finally, the proposed method was found to be simple and cost-effective, with adequate analytical performance for the rapid detection of Ni(II) in river and wastewater samples.

  11. Combination of solvent extractants for dispersive liquid-liquid microextraction of fungicides from water and fruit samples by liquid chromatography with tandem mass spectrometry.

    Science.gov (United States)

    Pastor-Belda, Marta; Garrido, Isabel; Campillo, Natalia; Viñas, Pilar; Hellín, Pilar; Flores, Pilar; Fenoll, José

    2017-10-15

    A multiresidue method was developed to determine twenty-five fungicides belonging to three different chemical families, oxazoles, strobilurins and triazoles, in water and fruit samples, using dispersive liquid-liquid microextraction (DLLME) and liquid chromatography/tandem mass spectrometry (LC-MS 2 ). Solid-liquid extraction with acetonitrile was used for the analysis in fruits, the extract being used as dispersant solvent in DLLME. Since some of the analytes showed high affinity for chloroform and the others were more efficiently extracted with undecanol, a mixture of both solvents was used as extractant in DLLME. After evaporation of CHCl 3 , the enriched phase was analyzed. Enrichment factors in the 23-119 and 12-60 ranges were obtained for waters and fruits, respectively. The approach was most sensitive for metominostrobin with limits of quantification of 1ngL -1 and 5ngkg -1 in waters and fruits, respectively, while a similar sensitivity was attained for tebuconazole in fruits. Recoveries of the fungicides varied between 86 and 116%. Copyright © 2017 Elsevier Ltd. All rights reserved.

  12. Temperature-controlled liquid-liquid microextraction combined with high-performance liquid chromatography for the simultaneous determination of diazinon and fenitrothion in water and fruit juice samples.

    Science.gov (United States)

    Bazmandegan-Shamili, Alireza; Dadfarnia, Shayessteh; Shabani, Ali Mohammad Haji; Moghadam, Masoud Rohani; Saeidi, Mahboubeh

    2018-02-28

    A simple, environmentally benign, and rapid method based on temperature-controlled liquid-liquid microextraction using a deep eutectic solvent was developed for the simultaneous extraction/preconcentration of diazinon and fenitrothion. The method involved the addition of deep eutectic solvent to the aqueous sample followed by heating the mixture in a 75°C water bath until the solvent was completely dissolved in the aqueous phase. Then, the resultant solution was cooled in an ice bath and a cloudy solution was formed. Afterward, the mixture was centrifuged and the enriched deep eutectic solvent phase was analyzed by high-performance liquid chromatography with ultraviolet detection for quantification of the analytes. The factors affecting the extraction efficiency were optimized. Under the optimized extraction conditions, the limits of detection for diazinon and fenitrothion were 0.3 and 0.15 μg/L, respectively. The calibration curves for diazinon and fenitrothion exhibited linearity in the concentration range of 1-100 and 0.5-100 μg/L, respectively. The relative standard deviations for five replicate measurements at 10.0 μg/L level of analytes were less than 2.8 and 4.5% for intra- and interday assays, respectively. The developed method was successfully applied to the determination of diazinon and fenitrothion in water and fruit juice samples. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Facile and sensitive determination of N-nitrosamines in food samples by high-performance liquid chromatography via combining fluorescent labeling with dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Lu, Shuaimin; Wu, Di; Li, Guoliang; Lv, Zhengxian; Gong, Peiwei; Xia, Lian; Sun, Zhiwei; Chen, Guang; Chen, Xuefeng; You, Jinmao; Wu, Yongning

    2017-11-01

    The intake of N-nitrosamines (NAs) from foodstuffs is considered to be an important influence factor for several cancers. But the rapid and sensitive screening of NAs remains a challenge in the field of food safety. Inspired by that, a sensitive and rapid method was demonstrated for determination of five NAs (Nitrosopyrrolidine, Nitrosodimethylamine, Nitrosodiethylamine, Nitrosodipropylamine and Nitrosodibutylamine) using dispersive liquid-liquid microextraction (DLLME) followed by high-performance liquid chromatography with fluorescence detection (HPLC-FLD). The NAs were firstly denitrosated and labeled by 2-(11H-benzo[a]carbazol-11-yl) ethyl carbonochloridate (BCEC-Cl) and finally enriched by DLLME. Furthermore, the main DLLME conditions were optimized systematically. Under the optimal conditions, satisfactory limits of detection (LODs) were obtained with a range of 0.01-0.07ngg -1 , which were significantly lower than the reported methods. The developed method showed many merits including rapidity, simplicity, high sensitivity and excellent selectivity, which shows a broad prospect in food safety analysis. Copyright © 2017 Elsevier Ltd. All rights reserved.

  14. Simultaneous determination of simazine, cyanazine, and atrazine in honey samples by dispersive liquid-liquid microextraction combined with high-performance liquid chromatography.

    Science.gov (United States)

    Tian, Hongzhe; Bai, Xuesong; Xu, Jing

    2017-10-01

    A rapid and simple sample preparation method was developed for simultaneous determination of three triazine herbicides in honey samples. The selected herbicides were extracted from honey samples by ionic liquid dispersive liquid-liquid microextraction, separated on a C 18 column (250 mm × 4.6 mm id, 5 μm) using acetonitrile and H 2 O as the mobile phase with gradient elution, and then detected by high-performance liquid chromatography. The parameters, such as the type and volume of the extraction and disperser solvent, ion strength, pH, extraction time, and centrifuge time were optimized in order to provide the excellent extraction performance. Good linearity was showed for all the target herbicides over the tested concentration range with correlation coefficient higher than 0.994. Three spiked levels (0.005, 0.05, 0.10 mg/kg) were applied for determination of the recoveries of the targets in honey samples in the range of 80-103% with relative standard deviations not larger than 10.6%. The limits of quantification for the analytes ranged between 1.5 and 4.0 μg/kg. The developed method was applied for determination of the target compounds residues in real samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Ultrasound-assisted ionic liquid dispersive liquid-liquid microextraction combined with graphite furnace atomic absorption spectrometric for selenium speciation in foods and beverages.

    Science.gov (United States)

    Tuzen, Mustafa; Pekiner, Ozlem Zeynep

    2015-12-01

    A rapid and environmentally friendly ultrasound assisted ionic liquid dispersive liquid liquid microextraction (USA-IL-DLLME) was developed for the speciation of inorganic selenium in beverages and total selenium in food samples by using graphite furnace atomic absorption spectrometry. Some analytical parameters including pH, amount of complexing agent, extraction time, volume of ionic liquid, sample volume, etc. were optimized. Matrix effects were also investigated. Enhancement factor (EF) and limit of detection (LOD) for Se(IV) were found to be 150 and 12 ng L(-1), respectively. The relative standard deviation (RSD) was found 4.2%. The accuracy of the method was confirmed with analysis of LGC 6010 Hard drinking water and NIST SRM 1573a Tomato leaves standard reference materials. Optimized method was applied to ice tea, soda and mineral water for the speciation of Se(IV) and Se(VI) and some food samples including beer, cow's milk, red wine, mixed fruit juice, date, apple, orange, grapefruit, egg and honey for the determination of total selenium. Copyright © 2015 Elsevier Ltd. All rights reserved.

  16. Zeolite imidazolate frameworks 8 as sorbent and its application to sonication-assisted emulsification microextraction combined with vortex-assisted porous membrane-protected micro-solid-phase extraction for fast analysis of acidic drugs in environmental water samples.

    Science.gov (United States)

    Ge, Dandan; Lee, Hian Kee

    2012-09-28

    A novel and fast procedure, sonication-assisted emulsification microextraction combined with vortex-assisted porous membrane protected micro-solid-phase extraction (SAEME-VA-μ-SPE), was developed for the gas chromatography-mass spectrometric determination of acidic drugs from environmental water samples. One advantage of the new procedure is that any solvent immiscible with water can be used as extractant solvent of SAEME and any solid sorbent can be used for μ-SPE in the SAEME-VA-μ-SPE process. In the present work, zeolite imidazolate framework 8 (ZIF-8) was employed as extraction sorbent for μ-SPE and 1-octanol as extractant solvent for SAEME. ZIF-8 has very good thermal, chemical and water stability, which make it a suitable material for the extraction of trace analytes from aqueous samples. Under the optimized extraction conditions, the developed method exhibited low limits of detection (0.01-0.04 ng/ml), good linearity (with r² between 0.9965 and 0.9993) from 0.5 to 50 ng/ml and satisfactory repeatability (between 4.1% and 7.6%). In essence SAEME-VA-μ-SPE is a combination of two different and efficient miniaturized techniques. It was demonstrated to be a fast, accurate, and convenient pretreatment procedure for trace analysis of environmental water samples. Copyright © 2012 Elsevier B.V. All rights reserved.

  17. Preliminary construction of integral analysis for characteristic components in complex matrices by in-house fabricated solid-phase microextraction fibers combined with gas chromatography-mass spectrometry.

    Science.gov (United States)

    Tang, Zhentao; Hou, Wenqian; Liu, Xiuming; Wang, Mingfeng; Duan, Yixiang

    2016-08-26

    Integral analysis plays an important role in study and quality control of substances with complex matrices in our daily life. As the preliminary construction of integral analysis of substances with complex matrices, developing a relatively comprehensive and sensitive methodology might offer more informative and reliable characteristic components. Flavoring mixtures belonging to the representatives of substances with complex matrices have now been widely used in various fields. To better study and control the quality of flavoring mixtures as additives in food industry, an in-house fabricated solid-phase microextraction (SPME) fiber was prepared based on sol-gel technology in this work. The active organic component of the fiber coating was multi-walled carbon nanotubes (MWCNTs) functionalized with hydroxyl-terminated polydimethyldiphenylsiloxane, which integrate the non-polar and polar chains of both materials. In this way, more sensitive extraction capability for a wider range of compounds can be obtained in comparison with commercial SPME fibers. Preliminarily integral analysis of three similar types of samples were realized by the optimized SPME-GC-MS method. With the obtained GC-MS data, a valid and well-fit model was established by partial least square discriminant analysis (PLS-DA) for classification of these samples (R2X=0.661, R2Y=0.996, Q2=0.986). The validity of the model (R2=0.266, Q2=-0.465) has also approved the potential to predict the "belongingness" of new samples. With the PLS-DA and SPSS method, further screening out the markers among three similar batches of samples may be helpful for monitoring and controlling the quality of the flavoring mixtures as additives in food industry. Conversely, the reliability and effectiveness of the GC-MS data has verified the comprehensive and efficient extraction performance of the in-house fabricated fiber. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. Dispersive micro-solid phase extraction combined with dispersive liquid-liquid microextraction for speciation analysis of antimony by electrothermal vaporization inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Chen, Shizhong; Zhu, Shengping; Lu, Dengbo

    2018-01-01

    A method was developed for speciation analysis of antimony by electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS) after preconcentration/separation using dispersive micro-solid phase extraction (DMSPE) and dispersive liquid-liquid micro-extraction (DLLME). In DMSPE, titanium dioxide nanofibers were used for preconcentration and separation of analytes. The upper aqueous phase and elution solution from DMSPE were used for further preconcentration and separation of Sb(III) and Sb(V) by DLLME without any pre-oxidation or pre-reduction operation, respectively. The extracts from DLLME were used for ETV-ICP-MS determination with APDC as a chemical modifier. Under optimal conditions, the detection limits of this method were 0.019 and 0.025 pg mL- 1 with relative standard deviations of 5.7% and 6.9% for Sb(III) and Sb(V) (c = 1.0 ng mL- 1, n = 9), respectively. This method was applied for speciation analysis of Sb and its distribution in the tea leaves and the tea infusion, including total, suspended, soluble, organic and inorganic Sb as well as Sb(III) and Sb(V). The results showed that the contents of Sb are 62.7, 12.9 and 47.3 ng g- 1 in the tea leaves, tea residue and tea soup, respectively; those of soluble, organic, inorganic, Sb(III) and Sb(V) are 0.41, 0.11, 0.29, 0.21 and 0.07 ng mL- 1 in the tea soup, respectively. A certified reference material of tea leaves (GBW 07605) was analyzed by this method with satisfactory results.

  19. A powerful methodological approach combining headspace solid phase microextraction, mass spectrometry and multivariate analysis for profiling the volatile metabolomic pattern of beer starting raw materials.

    Science.gov (United States)

    Gonçalves, João L; Figueira, José A; Rodrigues, Fátima P; Ornelas, Laura P; Branco, Ricardo N; Silva, Catarina L; Câmara, José S

    2014-10-01

    The volatile metabolomic patterns from different raw materials commonly used in beer production, namely barley, corn and hop-derived products - such as hop pellets, hop essential oil from Saaz variety and tetra-hydro isomerized hop extract (tetra hop), were established using a suitable analytical procedure based on dynamic headspace solid-phase microextraction (HS-SPME) followed by thermal desorption gas chromatography-quadrupole mass spectrometry detection (GC-qMS). Some SPME extraction parameters were optimized. The best results, in terms of maximum signal recorded and number of isolated metabolites, were obtained with a 50/30 μm DVB/CAR/PDMS coating fiber at 40 °C for 30 min. A set of 152 volatile metabolites comprising ketones (27), sesquiterpenes (26), monoterpenes (19), aliphatic esters (19), higher alcohols (15), aldehydes (11), furan compounds (11), aliphatic fatty acids (9), aliphatic hydrocarbons (8), sulphur compounds (5) and nitrogen compounds (2) were positively identified. Each raw material showed a specific volatile metabolomic profile. Monoterpenes in hop essential oil and corn, sesquiterpenes in hop pellets, ketones in tetra hop and aldehydes and sulphur compounds in barley were the predominant chemical families in the targeted beer raw materials. β-Myrcene was the most dominant volatile metabolite in hop essential oil, hop pellets and corn samples while, in barley, the predominant volatile metabolites were dimethyl sulphide and 3-methylbutanal and, in tetra hop, 6-methyl-2-pentanone and 4-methyl-2-pentanone. Principal component analysis (PCA) showed natural sample grouping among beer raw materials. Copyright © 2014 Elsevier Ltd. All rights reserved.

  20. Low-cost approach to increase the analysis throughput of bar adsorptive microextraction (BAµE) combined with environmentally-friendly renewable sorbent phase of recycled diatomaceous earth.

    Science.gov (United States)

    Mafra, Gabriela; Oenning, Anderson Luiz; Dias, Adriana Neves; Merib, Josias; Budziak, Dilma; Silveira, Cristian Berto da; Carasek, Eduardo

    2018-02-01

    In this study, a novel apparatus for bar adsorptive microextraction (BAµE) using a voltage regulator was proposed as an alternative tool to improve the analysis throughput. In addition, recycled diatomaceous earth obtained as a brewery residue was employed as a biosorbent coating for the determination of methyl paraben, ethyl paraben, benzophenone and triclocarban in water samples by high-performance liquid chromatography-diode array detection (HPLC-DAD). The use of the extraction devices, comprised of floating adsorptive bars of 7.5mm length, in the extractions with magnetic stirrers linked to a voltage regulator enabled the analysis of multiple samples, simultaneously. The method optimization was carried out by univariate and multivariate analyses. The optimal conditions for the method were sample solution at pH 5, extraction time of 90min and liquid desorption in 100µL of acetonitrile:methanol (50:50, v/v) for 15min. The total sample preparation time was 17.5min per sample for a simultaneous batch of six extractions. The R 2 values for the calibration curves obtained were higher than 0.9985. The limits of detection (LODs) varied from 0.19 to 2μgL -1 and the limits of quantification (LOQs) ranged from 0.63 to 6.9μgL -1 . The method was applied to freshwater samples collected from Peri Lagoon (Florianópolis, SC, Brazil) and the relative recoveries ranged from 63% to 124% with relative standard deviations (RSDs) of < 20% (n = 2). The RSD values for the reproducibility of the performance of the magnetic stirrers and inter-device extraction efficiency were lower than 14% (n = 3) and 11% (n = 3), respectively. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. Headspace solid-phase microextraction (HS-SPME) combined with GC-MS as a process analytical technology (PAT) tool for monitoring the cultivation of C. tetani.

    Science.gov (United States)

    Ghader, Masoud; Shokoufi, Nader; Es-Haghi, Ali; Kargosha, Kazem

    2018-02-06

    Vaccine production is a biological process in which variation in time and output is inevitable. Thus, the application of Process Analytical Technologies (PAT) will be important in this regard. Headspace solid - phase microextraction (HS-SPME) coupled with GC-MS can be used as a PAT for process monitoring. This method is suitable to chemical profiling of volatile organic compounds (VOCs) emitted from microorganisms. Tetanus is a lethal disease caused by Clostridium tetani (C. tetani) bacterium and vaccination is an ultimate way to prevent this disease. In this paper, SPME fiber was used for the investigation of VOCs emerging from C. tetani during cultivation. Different types of VOCs such as sulfur-containing compounds were identified and some of them were selected as biomarkers for bioreactor monitoring during vaccine production. In the second step, the portable dynamic air sampling (PDAS) device was used as an interface for sampling VOCs by SPME fibers. The sampling procedure was optimized by face-centered central composite design (FC-CCD). The optimized sampling time and inlet gas flow rates were 10 min and 2 m L s -1 , respectively. PDAS was mounted in exhausted gas line of bioreactor and 42 samples of VOCs were prepared by SPME fibers in 7 days during incubation. Simultaneously, pH and optical density (OD) were evaluated to cultivation process which showed good correlations with the identified VOCs (>80%). This method could be used for VOCs sampling from off-gas of a bioreactor to monitoring of the cultivation process. Copyright © 2018. Published by Elsevier B.V.

  2. In situ metathesis reaction combined with liquid-phase microextraction based on the solidification of sedimentary ionic liquids for the determination of pyrethroid insecticides in water samples.

    Science.gov (United States)

    Hu, Lu; Zhang, Panjie; Shan, Wanyu; Wang, Xuan; Li, Songqing; Zhou, Wenfeng; Gao, Haixiang

    2015-11-01

    A novel dispersion liquid-liquid microextraction method based on the solidification of sedimentary ionic liquids (SSIL-DLLME), in which an in situ metathesis reaction forms an ionic liquid (IL) extraction phase, was developed to determine four pyrethroid insecticides (i.e., permethrin, cyhalothrin, fenpropathrin, and transfluthrin) in water followed by separation using high-performance liquid chromatography. In the developed method, in situ DLLME was used to enhance the extraction efficiency and yield. After centrifugation, the extraction solvent, tributyldodecylphosphonium hexafluorophosphate ([P44412][PF6]), was easily collected by solidification in the bottom of the tube. The effects of various experimental parameters, the quantity of tributyldodecylphosphonium bromide ([P44412]Br), the molar ratio of [P44412]Br to potassium hexafluorophosphate (KPF6), the ionic strength, the temperature of the sample solution, and the centrifugation time, were optimized using a Plackett-Burman design to identify the significant factors that affected the extraction efficiency. These significant factors were then optimized using a central composite design. Under the optimized conditions, the recoveries of the four pyrethroid insecticides at four spiked levels ranged from 87.1% to 101.7%, with relative standard deviations (RSDs) ranging from 0.1% to 5.5%. At concentration levels between 1 and 500 µg/L, good linearity was obtained, with coefficients of determination greater than 0.9995. The limits of detection (LODs) for the four pyrethroid insecticides were in the range of 0.71-1.54 µg/L. The developed method was then successfully used for the determination of pyrethroid insecticides in environmental samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  3. Iron species determination by task-specific ionic liquid-based in situ solvent formation dispersive liquid-liquid microextraction combined with flame atomic absorption spectrometry.

    Science.gov (United States)

    Sadeghi, Susan; Ashoori, Vahid

    2017-10-01

    The task-specific ionic liquid (TSIL) of 1-ethyl-3-methylimidazolium bromide functionalized with 8-hydroxyquinoline was used as a chelating agent and extracting solvent for dispersive liquid-liquid microextraction and subsequent determination of Fe(III) by flame atomic absorption spectrometry. The in situ solvent formation of TSIL using KPF 6 provided the desired water-immiscible ionic liquid. The total Fe concentration could be determined after pre-oxidation of Fe(II) to Fe(III). Various factors affecting the proposed extraction procedure were optimized. The proposed analytical conditions were: sample pH 5, TSIL amount 0.3% (w/v), KPF 6 amount 0.15% (w/v), anti-sticking 0.1% (w/v) and salt concentration 5% (w/v). Under optimal conditions, the linear dynamic ranges for Fe(III) and total Fe were 20-80 and 20-110 ng mL -1 , respectively, with a detection limit of 6.9 ng mL -1 for Fe(III) and relative standard deviation of 2.2%. The proposed method was successfully applied to the determination of trace Fe(III) in water (underground, tap, refined water and artificial sea water) and beverage (apple, tomato, and tea) samples. The developed method offers advantages such as simplicity, ease of operation, and extraction of Fe(III) from aqueous solutions without the use of organic solvent. It was successfully applied for iron speciation in different real samples. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

  4. Pressure Drop

    Science.gov (United States)

    Lawson, Mike

    2010-01-01

    Mike Lawson briefly discussed pressure drop for aerospace applications and presented short stories about adventures experienced while working at NASA and General Dynamics, including exposure to technologies like the Crew and Equipment Translation Aid (CETA) cart and the SWME.

  5. Foot Drop

    Science.gov (United States)

    ... is being done? The National Institute of Neurological Disorders and Stroke (NINDS) conducts research related to the neurological conditions that cause foot drop in its laboratories at the National ...

  6. Development of a new sample preparation method based on liquid-liquid-liquid extraction combined with dispersive liquid-liquid microextraction and its application on unfiltered samples containing high content of solids.

    Science.gov (United States)

    Farajzadeh, Mir Ali; Abbaspour, Maryam

    2017-11-01

    A new sample preparation method based on liquid-liquid-liquid extraction combined with dispersive liquid-liquid microextraction followed by gas chromatography-flame ionization detection has been reported for the extraction/preconcentration and determination of trace levels of twelve pesticide residues from different samples with high content of solids without filtration. This method consists of a three-phase system including an aqueous phase (sample solution), acetonitrile, and hexane. The extraction mechanism is based on different affinities of the substances from the sample matrices towards each of the involved phase, which provides a high selectivity to the process. In other words, interfering hydrophobic compounds are transferred into hexane and will not be present in the final extract. Furthermore, ionic and polar compounds are retained in the aqueous phase. Therefore, only semi-polar compounds such as the studied pesticides are extracted into acetonitrile. In this method, a homogeneous solution of the aqueous phase and acetonitrile (a water-soluble extraction solvent) forms two clearly separated phases in the presence of sodium sulfate (as a phase separation agent) and simultaneously the analytes are extracted into the fine droplets of the acetonitrile collected on the surface of the aqueous phase. To achieve high enrichment factors, the acetonitrile phase is mixed with 1,2-dibromoethane (as a preconcentration solvent) at µL-level to perform the following dispersive liquid-liquid microextraction procedure. Several parameters that can affect extraction efficiency including kind and volume of extraction solvent, type and concentration of phase separation agent, hexane volume, kind of preconcentration solvent, and ionic strength were studied and optimized. Under the optimal conditions, extraction recoveries were obtained in the range of 53-93% and the calibration curves were linear in wide ranges with correlation coefficients ≥ 0.9983. Intra- (n = 6) and

  7. Gas chromatography-mass spectrometry determination of polycyclic aromatic hydrocarbons in baby food using QuEChERS combined with low-density solvent dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Petrarca, Mateus Henrique; Godoy, Helena Teixeira

    2018-08-15

    A sensitive GC-MS method is reported for the determination of twelve polycyclic aromatic hydrocarbons (PAHs) in baby food. The sample preparation involves QuEChERS extraction combined with low-density solvent dispersive liquid-liquid microextraction (LDS-DLLME) and ultra-low temperature (-80 °C). Plackett-Burman screening design was employed to identify the main sample preparation variables that affect the extraction efficiency, such as the volume of toluene used in LDS-DLLME. The suitability of proposed method was verified by analytical selectivity, linearity in solvent and matrix-matched calibration curves and adequate recoveries (72-112%) and precision (RSD values ≤11%), under repeatability and within-laboratory reproducibility conditions. High analytical sensitivity was achieved for the monitoring of PAHs at the strict limit of 1 µg kg -1 fixed by the European Commission for baby foods. The validated method was applied to thirty-two commercial baby food samples, and the investigated PAHs were not detected in any sample. Copyright © 2018 Elsevier Ltd. All rights reserved.

  8. Headspace hollow fiber protected liquid-phase microextraction combined with gas chromatography-mass spectroscopy for speciation and determination of volatile organic compounds of selenium in environmental and biological samples.

    Science.gov (United States)

    Ghasemi, Ensieh; Sillanpää, Mika; Najafi, Nahid Mashkouri

    2011-01-21

    A simple and novel speciation method for the determination of volatile organic compounds of selenium (dimethylselenide (DMSe) and dimethyldiselenide (DMDSe) has been developed using a headspace hollow fiber protected liquid-phase microextraction (HS-HF-LPME) combined with capillary gas chromatography-mass spectrometry (GC-MS). The organic solvent impregnated in the pores and filled inside the porous hollow fiber membrane was used as an extraction interface in the HS-HF-LPME of the compounds. The effect of different variables on the extraction efficiency was studied simultaneously using an experimental design. The variables of interest in the HS-HF-LPME were sample volume, extraction time, temperature of sample solution, ionic strength, stirring rate and dwelling time. A Plackett-Burman design was performed for screening in order to determine the significant variables affecting the extraction efficiency. Then, the significant factors were optimized by a Box-Behnken design (BBD) and the response surface equations were derived. Under optimum conditions, preconcentration factors up to 1250 and 1170 were achieved for DMSe and DMDSe respectively. The detection limit and relative standard deviation (RSD) (n=5, c=50 μg L(-1)) for DMSe were 65 ng L(-1) and 4.8%, respectively. They were also obtained for DMDSe as 57 ng L(-1) and 3.9%, respectively. The developed technique was found to be applicable to spiked environmental and biological samples. Copyright © 2010 Elsevier B.V. All rights reserved.

  9. Combination of corona discharge ion mobility spectrometry with a novel reagent gas and two immiscible organic solvent liquid-liquid-liquid microextraction for analysis of clomipramine in biological samples.

    Science.gov (United States)

    Saraji, Mohammad; Bidgoli, Ali Akbar Hajialiakbari; Khayamian, Taghi; Moradmand, Ali

    2011-12-02

    A novel and sensitive method based on combination of two immiscible organic solvents hollow fiber-based liquid-liquid-liquid microextraction and corona discharge ion mobility spectrometry (HF-LLLME-CD-IMS) was employed for the analysis of clomipramine in human urine and plasma. The effect of formic, acetic and propionic acid as the reagent gas (dopant) on the corona discharge ion mobility signal was investigated. The influence of dopant amount was also studied. Optimum mass flow rates of the dopants were 3.7, 1.1 and 1.0 μmol min(-1) for formic, acetic and propionic acid, respectively. Experimental parameters influencing the extraction efficiency of HF-LLLME, such as NaOH concentration as donor solution, ionic strength of the sample, stirring rate, and extraction time were investigated and optimized. Under the optimum conditions, analytical parameters such as linearity, precision and limit of detection were also evaluated. The linear dynamic range was from 1 to 100 μg L(-1) (r(2)=0.9980) and the limit of detection was 0.35 μg L(-1). Intra- and inter-day precisions were satisfactory with a relative standard deviation (RSD) of 5.9 and 6.7%, respectively. The proposed method was satisfactorily applied for the determination of clomipramine in human plasma and urine. Copyright © 2011 Elsevier B.V. All rights reserved.

  10. Comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry combined with solid phase microextraction as a powerful tool for quantification of ethyl carbamate in fortified wines. The case study of Madeira wine.

    Science.gov (United States)

    Perestrelo, Rosa; Petronilho, Sílvia; Câmara, José S; Rocha, Sílvia M

    2010-05-14

    An analytical methodology based on headspace solid phase microextraction (HS-SPME) combined with comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry (GC x GC-ToFMS) was developed for the identification and quantification of the toxic contaminant ethyl carbamate (EC) directly in fortified wines. The method performance was assessed for dry/medium dry and sweet/medium sweet model wines, and for quantification purposes, calibration plots were performed for both matrices using the ion extraction chromatography (IEC) mode (m/z 62). Good linearity was obtained with a regression coefficient (r(2)) higher than 0.981. A good precision was attained (R.S.D. wines. The quantification limits (LOQ) and recovery for dry wines were 14.38 microg/L and 88.6%, whereas for sweet wines were 9.16 microg/L and 99.4%, respectively. The higher performance was attained with sweet model wine, as increasing of glucose content improves the volatile compound in headspace, and a better linearity, recovery and precision were achieved. The analytical methodology was applied to analyse 20 fortified Madeira wines including different types of wine (dry, medium dry, sweet, and medium sweet) obtained from several harvests in Madeira Island (Portugal). The EC levels ranged from 54.1 microg/L (medium dry) to 162.5 microg/L (medium sweet). 2010 Elsevier B.V. All rights reserved.

  11. Trace determination of antibacterial pharmaceuticals in fishes by microwave-assisted extraction and solid-phase purification combined with dispersive liquid-liquid microextraction followed by ultra-high performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Huang, Peiting; Zhao, Pan; Dai, Xinpeng; Hou, Xiaohong; Zhao, Longshan; Liang, Ning

    2016-02-01

    A novel pretreatment method involving microwave-assisted extraction and solid-phase purification combined with dispersive liquid-liquid microextraction (MAE-SPP-DLLME) followed by ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was established for the simultaneous determination of six antibacterial pharmaceuticals including metronidazole, tinidazole, chloramphenicol, thiamphenicol, malachite green and crystal violet. The conditions of MAE were optimized using an orthogonal design and the optimal conditions were found to be 8mL for acetonitrile, 50°C for 5min. Then, neutral alumina column was employed in the solid-phase purification. Finally, the critical parameters affecting DLLME, including selection of extraction and dispersive solvent, adjustment of pH, salt concentration, extraction time, were investigated by single factor study. Under optimum conditions, good linearities (r>0.9991) and satisfied recoveries (Recoveries>87.0%, relative standard deviation (RSD)extraction followed by purification. The established method was sensitive, rapid, accurate and employable to simultaneously determine target analytes in farmed fish, river fish and marine fish. Copyright © 2015 Elsevier B.V. All rights reserved.

  12. Deep eutectic solvent based gas-assisted dispersive liquid-phase microextraction combined with gas chromatography and flame ionization detection for the determination of some pesticide residues in fruit and vegetable samples.

    Science.gov (United States)

    Farajzadeh, Mir Ali; Sattari Dabbagh, Masoumeh; Yadeghari, Adeleh

    2017-05-01

    In this study, a gas-assisted dispersive liquid-phase microextraction method using a deep eutectic solvent as the extraction solvent combined with gas chromatography and flame ionization detection was developed for the extraction and determination of some pesticide residues in vegetable and fruit juice samples. In this method, choline chloride and 4-chlorophenol at a molar ratio of 1:2 were mixed. By heating and vortexing, a clear, water-immiscible, and homogeneous liquid was formed. The obtained deep eutectic solvent was added to an aqueous solution of the analytes in a conical test tube. Air was bubbled into the aqueous solution and a cloudy solution was obtained. During this step, the analytes were extracted into the fine droplets of the extraction solvent. After centrifugation, an aliquot of the settled phase was injected into the separation system. Under the optimum extraction conditions, enrichment factors, and extraction recoveries were obtained in the ranges of 247-355 and 49-71%, respectively. The obtained values for the limits of detection and quantification were in the ranges of 0.24-1.4 and 0.71-4.2 μg/L, respectively. The proposed method is simple, fast, efficient, and inexpensive. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Assessment of the ventilation function and serum biochemical indexes after sublingual dermatophagoides farinae drops combined with loratadine treatment of children with asthma and allergic rhinitis

    Directory of Open Access Journals (Sweden)

    Ruo-Qing Qiu

    2017-06-01

    Full Text Available Objective: To study the ventilation function after sublingual dermatophagoides farinae drops combined with loratadine treatment of children with asthma and allergic rhinitis and the influence on serum biochemical indexes. Methods: A total of 40 children with asthma and allergic rhinitis treated in our hospital between September 2013 and March 2015 were collected and divided into the control group (n=22 who accepted loratadine therapy alone and the observation group (n=18 who accepted sublingual dermatophagoides farinae drops combined with loratadine therapy after the treatment was reviewed. Before treatment and after 6 months and 1 year of treatment, spirometer was used to test ventilation function indexes; ELISA method was used to determine the contents of inflammatory mediators; RIA method was used to determine the contents of airway remodeling indicators. Results: Before treatment, differences in ventilation function index levels as well as inflammatory mediator and airway remodeling index contents were not statistically significant between two groups of children. After 6 months and 1 year of treatment, FEV1, FVC and PEF levels of observation group were higher than those of control group; serum IL-2 content was higher than that of control group while IL-5, IL-17 and IL-33 contents were lower than those of control group; serum PDGFBB, TGF-β1 and NF-κB contents were lower than those of control group. Conclusion: Sublingual dermatophagoides farinae drops combined with loratadine therapy can optimize the ventilation function, reduce the systemic inflammatory response and inhibit airway remodeling in children with asthma and allergic rhinitis.

  14. Solid phase microextraction.

    Science.gov (United States)

    Pawliszyn, J

    2001-01-01

    Solid Phase Microextraction (SPME) uses a small volume of sorbent dispersed typically on the surface of small fibres, to isolate and concentrate analytes from sample matrix. After contact with sample, analytes are absorbed or adsorbed by the fibre phase (depending on the nature of the coating) until an equilibrium is reached in the system. The amount of an analyte extracted by the coating at equilibrium is determined by the magnitude of the partition coefficient of the analyte between the sample matrix and the coating material. After the extraction step, the fibres are transferred, with the help of a syringe-like handling device, to analytical instrument, for separation and quantitation of target analytes. This technique integrates sampling, extraction and sample introduction and is a simple way of facilitating on-site monitoring. Applications of this technique include environmental monitoring, industrial hygiene, process monitoring, clinical, forensic, food, flavour, fragrance and drug analyses, in laboratory and on-site analysis.

  15. Ionic-liquid-based dispersive liquid-liquid microextraction combined with magnetic solid-phase extraction for the determination of aflatoxins B1, B2, G1, and G2in animal feeds by high-performance liquid chromatography with fluorescence detection.

    Science.gov (United States)

    Zhao, Jiao; Zhu, Yan; Jiao, Yang; Ning, Jinyan; Yang, Yaling

    2016-10-01

    A novel two-step extraction technique combining ionic-liquid-based dispersive liquid-liquid microextraction with magnetic solid-phase extraction was developed for the preconcentration and separation of aflatoxins in animal feedstuffs before high-performance liquid chromatography coupled with fluorescence detection. In this work, ionic liquid 1-octyl-3-methylimidazolium hexafluorophosphate was used as the extractant in dispersive liquid-liquid microextraction, and hydrophobic pelargonic acid modified Fe 3 O 4 magnetic nanoparticles as an efficient adsorbent were applied to retrieve the aflatoxins-containing ionic liquid. Notably, the target of magnetic nanoparticles was the ionic liquid rather than the aflatoxins. Because of the rapid mass transfer associated with the dispersive liquid-liquid microextraction and magnetic solid phase steps, fast extraction could be achieved. The main parameters affecting the extraction recoveries of aflatoxins were investigated and optimized. Under the optimum conditions, vortexing at 2500 rpm for 1 min in the dispersive liquid-liquid microextraction and magnetic solid-phase extraction and then desorption by sonication for 2 min with acetonitrile as eluent. The recoveries were 90.3-103.7% with relative standard deviations of 3.2-6.4%. Good linearity was observed with correlation coefficients ranged from 0.9986 to 0.9995. The detection limits were 0.632, 0.087, 0.422 and 0.146 ng/mL for aflatoxins B 1 , B2, G1, and G2, respectively. The results were also compared with the pretreatment method carried out by conventional immunoaffinity columns. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Chlorophenol's ultra-trace analysis in environmental samples by chitosan-zinc oxide nanorod composite as a novel coating for solid phase micro-extraction combined with high performance liquid chromatography.

    Science.gov (United States)

    Alizadeh, Reza

    2016-01-01

    In this study, a simple, novel, and efficient preconcentration method has been developed for the determination of some chlorophenols (4-chlorophenol, 2,5-dichlorophenol, 2,3-dichlorophenol, and 2,4,6-trichlorophenol) using a direct solid phase microextraction (D-SPME) based on chitosan-ZnO nanorod composite combined with high performance liquid chromatography (HPLC). A one step-novel hydrothermal method was demonstrated on the fabrication of ZnO nanorods arrayed on the fused silica fiber in the chitosan hydrogel solution (CZNC) as a new coating of SPME fiber. The coating was characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD) instruments. The CZNC coating has combined the merits of both ZnO nanorods and chitosan hydrogel; it has several improvements such as increased extraction efficiency of chlorophenols and longer life time (over 80 cycles of D-SPME-HPLC operation). Experimental design method was used for optimization of extraction conditions and determination of four chlorophenols in water samples by SPME-HPLC-UV method. The calibration curves were linear from 5 to 1000 µg L(-1) for analytes, and the limits of detection were between 0.1 and 2 µg L(-1). Single fiber repeatability and fiber-to-fiber reproducibility were in the range of 5.8-10.2% and 8.8-14.5%, respectively. The spiked recoveries at 50 µg L(-1) for environmental water sample were in the range of 93-102%. Copyright © 2015 Elsevier B.V. All rights reserved.

  17. [Combined rapamycin eye drop in nanometer vector and poly (lactic acid) wafers of cyclosporine A effectively prevents high-risk corneal allograft rejection in rabbits].

    Science.gov (United States)

    Jiang, Wei; Sun, Hui-Min; Li, Xiao-Rong; Yuan, Xu-Bo; Wang, Yu-Qing; Zhang, Shu-Xian; Tian, En-Jiang; Yuan, Jia-Qin

    2009-06-01

    To evaluate the combined effect of topical rapamycin (RAPA) eye drop in nanometer vector and poly (lactic acid) (PLA) wafers of cyclosporine A (CsA) in the prevention of acute allograft rejection after rabbit corneal transplantation. Methods It was an experimental study. RAPA was incorporated into the nanometer particles and CsA was incorporated into PLA wafers. A was syngeneic control whose both donor and recipient are New Zealand rabbit. Gray donor corneas were implanted into the 102 recipients of New Zealand albino rabbits with corneal neovascularization who were randomly divided into B, C, D, E, F, G 6 groups to receive the different types of therapy: B was no therapy control; C was eye drop of nanometer vector but no RAPA twice a day, 28 days; D was PLA wafers in the anterior chamber of rabbit eyes but no drugs; E was 0.5% RAPA eye drop of nanometer vector twice a day, 28 days; F was PLA wafers of CsA in the anterior chamber of rabbit eyes; G was PLA wafers of CsA in the anterior chamber of rabbit eyes and 0.5% RAPA eye drop of nanometer vector eye drop twice a day for 28 days together. Postoperative evaluation included slit-lamp biomicroscopy, histopathology and immunohistology, Cytokines related with neovascularization and immunosuppression in the corneal tissue by RT-PCR. The graft survival was assessed by One-Way ANOVA and q test. Corneal allograft survival time: A (100.00 +/- 0.00), B (8.44 +/- 1.24), C (8.89 +/- 2.57), D (8.56 +/- 2.30), E (43.11 +/- 5.58), F (43.67 +/- 9.54), G (72.00 +/- 15.34) d. Group G led to a statistically significant prolongation of transplant survival and was superior than group E and F which was a statistical prolongation compared with group B, C and D (qGE = 11.42, qGF = 11.24, qEB = 13.64, qEC = 13.38, qED = 13.46, qFB = 13.82, qFC = 13.56, qFD = 13.64; P < 0.01). Immunohistopathologically, the grafts were subjected to an immune response contained a dense infiltrate of neutrophils, CD4+ and CD8+ T lymphocytes in the group B

  18. Development of magnetic dispersive solid phase extraction using toner powder as an efficient and economic sorbent in combination with dispersive liquid-liquid microextraction for extraction of some widely used pesticides in fruit juices.

    Science.gov (United States)

    Farajzadeh, Mir Ali; Mohebbi, Ali

    2018-01-12

    In this study, for the first time, a magnetic dispersive solid phase extraction method using an easy-accessible, cheap, and efficient magnetic sorbent (toner powder) combined with dispersive liquid-liquid microextraction has been developed for the extraction and preconcentration of some widely used pesticides (diazinon, ametryn, chlorpyrifos, penconazole, oxadiazon, diniconazole, and fenazaquin) from fruit juices prior to their determination by gas chromatography-flame ionization detection. In this method, the magnetic sorbent is mixed with an appropriate dispersive solvent (methanol-water, 80:20, v/v) and then injected into an aqueous sample containing the analytes. By this action the analytes are rapidly adsorbed on the sorbent by binding to its carbon. The sorbent particles are isolated from the aqueous solution in the presence of an external magnetic field. Then an appropriate organic solvent (acetone) is used to desorb the analytes from the sorbent. Finally, the obtained supernatant is mixed with an extraction solvent and injected into deionized water in order to achieve high enrichment factors and sensitivity. Several significant factors affecting the performance of the introduced method were investigated and optimized. Under the optimum experimental conditions, the extraction recoveries of the proposed method for the selected analytes ranged from 49-75%. The relative standard deviations were ≤7% for intra- (n = 6) and inter-day (n = 4) precisions at a concentration of 10 μg L -1 of each analyte. The limits of detection were in the range of 0.15-0.36 μg L -1 . Finally, the applicability of the proposed method was evaluated by analysis of the selected analytes in some fruit juices. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. Dynamic headspace solid-phase microextraction combined with one-dimensional gas chromatography-mass spectrometry as a powerful tool to differentiate banana cultivars based on their volatile metabolite profile.

    Science.gov (United States)

    Pontes, Marisela; Pereira, Jorge; Câmara, José S

    2012-10-15

    In this study the effect of the cultivar on the volatile profile of five different banana varieties was evaluated and determined by dynamic headspace solid-phase microextraction (dHS-SPME) combined with one-dimensional gas chromatography-mass spectrometry (1D-GC-qMS). This approach allowed the definition of a volatile metabolite profile to each banana variety and can be used as pertinent criteria of differentiation. The investigated banana varieties (Dwarf Cavendish, Prata, Maçã, Ouro and Platano) have certified botanical origin and belong to the Musaceae family, the most common genomic group cultivated in Madeira Island (Portugal). The influence of dHS-SPME experimental factors, namely, fibre coating, extraction time and extraction temperature, on the equilibrium headspace analysis was investigated and optimised using univariate optimisation design. A total of 68 volatile organic metabolites (VOMs) were tentatively identified and used to profile the volatile composition in different banana cultivars, thus emphasising the sensitivity and applicability of SPME for establishment of the volatile metabolomic pattern of plant secondary metabolites. Ethyl esters were found to comprise the largest chemical class accounting 80.9%, 86.5%, 51.2%, 90.1% and 6.1% of total peak area for Dwarf Cavendish, Prata, Ouro, Maçã and Platano volatile fraction, respectively. Gas chromatographic peak areas were submitted to multivariate statistical analysis (principal component and stepwise linear discriminant analysis) in order to visualise clusters within samples and to detect the volatile metabolites able to differentiate banana cultivars. The application of the multivariate analysis on the VOMs data set resulted in predictive abilities of 90% as evaluated by the cross-validation procedure. Copyright © 2012 Elsevier Ltd. All rights reserved.

  20. Persistent sample circulation microextraction combined with graphite furnace atomic absorption spectroscopy for trace determination of heavy metals in fish species marketed in Kermanshah, Iran, and human health risk assessment.

    Science.gov (United States)

    Safari, Yahya; Karimaei, Mostafa; Sharafi, Kiomars; Arfaeinia, Hossein; Moradi, Masoud; Fattahi, Nazir

    2017-11-21

    Persistent sample circulation microextraction (PSCME) combined with graphite furnace atomic absorption spectrometry (GFAAS) was developed as a high pre-concentration technique for the determination of heavy metals in fish species. In this method, a few microliters of organic solvent (40.0 µL carbon tetrachloride) was transferred to the bottom of a conical sample cup. Then 10.0 mL of aqueous solution was transformed to fine droplets while passing through the organic solvent. At this stage, metal-ligand hydrophobic complex was extracted into the organic solvent. After extraction, 20 µL of extraction solvent was injected into the graphite tube using an auto-sampler. Under optimal conditions, enrichment factors and enhancement factor were in the range of 180-240 and 155-214, respectively. The calibration curves were linear in the range of 0.03-200 µg kg -1 and the limits of detection (LODs) were in the range of 0.01-0.05 µg kg -1 . Repeatability (intra-day) and reproducibility (inter-day) for 0.50 µg L -1 Hg and 0.10 µg L -1 Cd and Pb were in the range of 3.1-4.2% (n = 7) and 4.3-6.1% (n = 7), respectively. Potential human health risk assessment was conducted by calculating estimated weekly intake (EWI) of the metals from eating fish and comparison of these values with provisional tolerable weekly intake (PTWI) values. EWI data for the studied metals through fish consumption were lower than the PTWI values. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

  1. Determination of fluoroquinolone antibiotics via ionic-liquid-based, salt-induced, dual microextraction in swine feed.

    Science.gov (United States)

    Wang, Huili; Gao, Ming; Gao, Jiajia; Yu, Nana; Huang, Hong; Yu, Qing; Wang, Xuedong

    2016-09-01

    In conventional microextraction procedures, the disperser (organic solvent or ionic liquid) is left in the aqueous phase and discarded after finishing the microextraction process. Because the disperser is water-soluble, it results in low extraction recovery for polar compounds. In this investigation, an ionic-liquid-based microextraction (ILBME) was integrated with salting-out assisted liquid-liquid microextraction (SALLME) to build an ionic-liquid-based, salt-induced, dual microextraction (ILSDME) for isolation of five fluoroquinolone antibiotics (FQs) with high polarity (log P, -1.0 to 1.0). The proposed ILSDME method incorporates a dual microextraction by converting the disperser in the ILBME to the extractor in the SALLME. Optimization of key factors was conducted by integrating single-factor experiments and central composite design. The optimized experimental parameters were 80 μL [C8MIM][PF6] as extractor, 505 μL acetone as disperser, pH = 2.0, 4.1 min extraction time, and 4.2 g of Na2SO4. Under optimized conditions, high ERs (90.6-103.2 %) and low LODs (0.07-0.61 μg kg(-1)) were determined for five FQs in swine feed. Experimental precision based on RSDs was 1.4-5.2 % for intra-day and 2.4-6.9 % for inter-day analyses. The combination of ILBME with SALLME increased FQ recoveries by 15-20 % as compared with SALLME, demonstrating that the ILSDME method can enhance extraction efficiency for polar compounds compared to single-step microextraction. Therefore, the ILSDME method developed in this study has wide application for pretreatment of moderately to highly polar pollutants in complex matrices. Graphical Abstract A dual microextraction was developed by integrating ionic-liquid-based microextraction with salting-out assisted liquid-liquid microextraction for isolation of five fluoroquinolone antibiotics (FQs) with high polarity (log P = -1.0 to 1.0). The principle of dual microextraction is based on converting the remaining disperser from

  2. Ultrasound-assisted ionic liquid-based micellar extraction combined with microcrystalline cellulose as sorbent in dispersive microextraction for the determination of phenolic compounds in propolis.

    Science.gov (United States)

    Cao, Jun; Peng, Li-Qing; Du, Li-Jing; Zhang, Qi-Dong; Xu, Jing-Jing

    2017-04-22

    An ionic liquid-(IL) based micellar extraction combined with microcrystalline cellulose- (MCC) assisted dispersive micro solid-phase extraction method was developed to extract phenolic compounds from propolis. A total of 20 target compounds were identified by ultra-high- performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry. The main extraction parameters were optimized and included the ultrasonic power, ultrasonic time, sample pH, type of IL, the concentration of [C12mim]Br, extraction time, concentration of MCC, type of sorbent and type of elution solvents. Under the optimum conditions, the proposed method exhibited good linearities (r 2  ≥ 0.999) for all plant phenolic compounds with the lower limits of detection in the range of 0.21-0.41 ng/mL. The recoveries ranged from 82.74% to 97.88% for pinocembrin, chrysin and galangin. Compared with conventional solvent extraction, the present method was simpler and more efficient and required less organic solvent and a shorter extraction time. Finally, the methodology was successfully used for the extraction and enrichment of phenolic compounds in propolis. Copyright © 2017 Elsevier B.V. All rights reserved.

  3. Dummy-surface molecularly imprinted polymers as a sorbent of micro-solid-phase extraction combined with dispersive liquid-liquid microextraction for determination of five 2-phenylpropionic acid NSAIDs in aquatic environmental samples.

    Science.gov (United States)

    Guo, Ping; Yuan, Xucan; Zhang, Jingjing; Wang, Binjie; Sun, Xiaoyang; Chen, Xiaohui; Zhao, Longshan

    2018-01-01

    their environmental fate and risk to ecological health. Graphical abstract Dummy-surface molecularly imprinted polymers as a sorbent of micro-solid-phase extraction combined with dispersive liquid-liquid microextraction for determination of five 2-phenylpropionic acid NSAIDs in aquatic environmental samples.

  4. Simultaneous determination of brazilin and protosappanin B in Caesalpinia sappan by ionic-liquid dispersive liquid-phase microextraction method combined with HPLC.

    Science.gov (United States)

    Xia, Zhaoyang; Li, Dongdong; Li, Qing; Zhang, Yan; Kang, Wenyi

    2017-11-13

    The conditions of heating, ionic liquid-based ultrasonic-assisted extraction combined with reverse-phase high performance liquid chromatography were optimized to simultaneously isolate and determinate brazilin and protosappanin B in Caesalpinia sappan. Ionic liquids, including [BMIM]Br, [BMIM]BF 4 , [BMIM]PF 6 and [HMIM]PF 6 , were selected as extraction solvents while methanol, acetone, acetonitrile, ethanol and water were selected as dispersants. The chromatographic column was Purospher star RP-C 18 (250 mm × 4.6 mm, 5 μm), a mixture of methanol and 0.2% phosphoric acid-water was used as mobile phase at a flow rate 0.65 mL/min. The result displayed that the extraction yields of brazilin and protosappanin B were highest when the concentration of [BMIM]Br methanol solution as extraction solvent was 0.5 mol/L and the solid-liquid ratio was 1:50 (g/mL). Under the optimal extraction conditions, the contents of brazilin showed a good linearity (r = 1.0000) within the range of 1.25-7.50 μg with the average recovery of 99.33%, the contents of protosappanin B also showed a good linearity (r = 0.9999) within the range of 0.50-3.00 μg with the average recovery of 98.31%. This experiment, which adopted environmentally friendly reagent as extraction solvent, not only improved the extraction efficiency, but also avoided the environmental pollution caused by organic solvent. Moreover, it was simple and reliable, and can be of important significance in the study of Traditional Chinese Medicine active ingredient extraction methods. The antibacterial activities of the ionic liquids and methanol extracts were determined using the paper disc diffusion method. The ionic liquid extract was found to possess antibacterial activity against Staphylococcus aureus and methicillin-resistant S. aureus (MIC value of 37.5 mg crude drug/mL), β-Lactamase producing S. aureus (MIC values of 18.8 mg crude drug/mL), but not against E. coli, Extended spectrum β-Lactamases E. coli

  5. Solid-phase microextraction

    DEFF Research Database (Denmark)

    Nilsson, Torben

    and organophosphate pesticides and triazine herbicides together with their metabolites in aqueous samples. SPME combined with gas chromatography proved to be a precise, accurate and sensitive technique for water analysis. Also SPME combined with high performance liquid chromatography was tested, and a method...

  6. Active connectors for microfluidic drops on demand

    Energy Technology Data Exchange (ETDEWEB)

    Galas, Jean-Christophe; Studer, Vincent [Laboratoire de Neurobiologie, ESPCI-CNRS UMR 7637, 10 rue Vauquelin 75231 Paris cedex 05 (France); Bartolo, Denis [PMMH-ESPCI-CNRS UMR 7636-Universite Paris 6-Universite Paris 7, 10 rue Vauquelin 75231 Paris cedex 05 (France)], E-mail: jean-christophe.galas@espci.fr, E-mail: denis.bartolo@espci.fr, E-mail: vincent.studer@espci.fr

    2009-07-15

    We introduce a simple and versatile microfluidic drop-on-demand solution that enables independent and dynamical control of both the drop size and the drop production rate. To do so, we combine a standard microfluidic T-junction and a novel active switching component that connects the microfluidic channel to the macroscopic liquid reservoirs. Firstly, we explain how to make this simple but accurate drop-on-demand device. Secondly, we carefully characterize its dynamic response and its range of operations. Finally, we show how to generate complex two-dimensional drop patterns dynamically in single or multiple synchronized drop-on-demand devices.

  7. Performance Analysis of an Evaporator for a Diesel Engine–Organic Rankine Cycle (ORC Combined System and Influence of Pressure Drop on the Diesel Engine Operating Characteristics

    Directory of Open Access Journals (Sweden)

    Chen Bei

    2015-06-01

    Full Text Available The main purpose of this research is to analyze the performance of an evaporator for the organic Rankine cycle (ORC system and discuss the influence of the evaporator on the operating characteristics of diesel engine. A simulation model of fin-and-tube evaporator of the ORC system is established by using Fluent software. Then, the flow and heat transfer characteristics of the exhaust at the evaporator shell side are obtained, and then the performance of the fin-and-tube evaporator of the ORC system is analyzed based on the field synergy principle. The field synergy angle (β is the intersection angle between the velocity vector and the temperature gradient. When the absolute values of velocity and temperature gradient are constant and β < 90°, heat transfer enhancement can be achieved with the decrease of the β. When the absolute values of velocity and temperature gradient are constant and β >90°, heat transfer enhancement can be achieved with the increase of the β. Subsequently, the influence of the evaporator of the ORC system on diesel engine performance is studied. A simulation model of the diesel engine is built by using GT–Power software under various operating conditions, and the variation tendency of engine power, torque, and brake specific fuel consumption (BSFC are obtained. The variation tendency of the power output and BSFC of diesel engine–ORC combined system are obtained when the evaporation pressure ranges from 1.0 MPa to 3.5 MPa. Results show that the field synergy effect for the areas among the tube bundles of the evaporator main body and the field synergy effect for the areas among the fins on the windward side are satisfactory. However, the field synergy effect in the areas among the fins on the leeward side is weak. As a result of the pressure drop caused by the evaporator of the ORC system, the diesel engine power and torque decreases slightly, whereas the BSFC increases slightly with the increase of exhaust back

  8. Application of dynamic liquid-phase microextraction and injection port derivatization combined with gas chromatography-mass spectrometry to the determination of acidic pharmaceutically active compounds in water samples.

    Science.gov (United States)

    Zhang, Jie; Lee, Hian Kee

    2009-10-30

    A method has been established for the determination of four pharmaceutically active compounds (ibuprofen, ketoprofen, naproxen and clofibric acid) in water samples using dynamic hollow fiber liquid-phase microextraction (HF/LPME) followed by gas chromatography (GC) injection port derivatization and GC-mass spectrometric (MS) determination. Dynamic HF/LPME is a novel approach to microextraction that involves the use of a programmable syringe pump to move the liquid phases participating in the extraction so as to facilitate the process. Trimethylanilinium hydroxide (TMAH) was used as derivatization reagent for the analytes to increase their volatility and improve chromatographic separation. Parameters that affect extraction efficiency (selection of organic solvent, volume of organic solvent, agitation in the donor phase, plunger movement and extraction time) were investigated. Under optimal conditions, the proposed method provided good enrichment factors up to 251, reproducibility ranging from 3.26% to 10.61%, and good linearity from 0.2 to 50 microg/L. The limits of detection ranged between 0.01 and 0.05 microg/L (S/N=3) using selective ion monitoring. This method was applied to the determination of the four pharmaceutically active compounds in tap water and wastewater collected from a drain in the vicinity of a hospital.

  9. A new combined method of stable isotope-labeling derivatization-ultrasound-assisted dispersive liquid-liquid microextraction for the determination of neurotransmitters in rat brain microdialysates by ultra high performance liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Zheng, Longfang; Zhao, Xian-En; Zhu, Shuyun; Tao, Yanduo; Ji, Wenhua; Geng, Yanling; Wang, Xiao; Chen, Guang; You, Jinmao

    2017-06-01

    In this work, for the first time, a new hyphenated technique of stable isotope-labeling derivatization-ultrasound-assisted dispersive liquid-liquid microextraction has been developed for the simultaneous determination of monoamine neurotransmitters (MANTs) and their biosynthesis precursors and metabolites. The developed method was based on ultra high performance liquid chromatography tandem mass spectrometry detection using multiple-reaction monitoring mode. A pair of mass spectrometry sensitizing reagents, d 0 -10-methyl-acridone-2-sulfonyl chloride and d 3 -10-methyl-acridone-2-sulfonyl chloride, as stable isotope probes was utilized to facilely label neurotransmitters, respectively. The heavy labeled MANTs standards were prepared and used as internal standards for quantification to minimize the matrix effects in mass spectrometry analysis. Low toxic bromobenzene (extractant) and acetonitrile (dispersant) were utilized in microextraction procedure. Under the optimized conditions, good linearity was observed with the limits of detection (S/N>3) and limits of quantification (S/N>10) in the range of 0.002-0.010 and 0.015-0.040nmol/L, respectively. Meanwhile, it also brought acceptable precision (4.2-8.8%, peak area RSDs %) and accuracy (recovery, 96.9-104.1%) results. This method was successfully applied to the simultaneous determination of monoamine neurotransmitters and their biosynthesis precursors and metabolites in rat brain microdialysates of Parkinson's disease and normal rats. This provided a new method for the neurotransmitters related studies in the future. Copyright © 2017 Elsevier B.V. All rights reserved.

  10. Dilating Eye Drops

    Science.gov (United States)

    ... Frequently Asked Questions Español Condiciones Chinese Conditions Dilating Eye Drops En Español Read in Chinese What are dilating eye drops? Dilating eye drops contain medication to enlarge ( ...

  11. Introducing a new and rapid microextraction approach based on magnetic ionic liquids: Stir bar dispersive liquid microextraction.

    Science.gov (United States)

    Chisvert, Alberto; Benedé, Juan L; Anderson, Jared L; Pierson, Stephen A; Salvador, Amparo

    2017-08-29

    With the aim of contributing to the development and improvement of microextraction techniques, a novel approach combining the principles and advantages of stir bar sorptive extraction (SBSE) and dispersive liquid-liquid microextraction (DLLME) is presented. This new approach, termed stir bar dispersive liquid microextraction (SBDLME), involves the addition of a magnetic ionic liquid (MIL) and a neodymium-core magnetic stir bar into the sample allowing the MIL coat the stir bar due to physical forces (i.e., magnetism). As long as the stirring rate is maintained at low speed, the MIL resists rotational (centrifugal) forces and remains on the stir bar surface in a manner closely resembling SBSE. By increasing the stirring rate, the rotational forces surpass the magnetic field and the MIL disperses into the sample solution in a similar manner to DLLME. After extraction, the stirring is stopped and the MIL returns to the stir bar without the requirement of an additional external magnetic field. The MIL-coated stir bar containing the preconcentrated analytes is thermally desorbed directly into a gas chromatographic system coupled to a mass spectrometric detector (TD-GC-MS). This novel approach opens new insights into the microextraction field, by using the benefits provided by SBSE and DLLME simultaneously, such as automated thermal desorption and high surface contact area, respectively, but most importantly, it enables the use of tailor-made solvents (i.e., MILs). To prove its utility, SBDLME has been used in the extraction of lipophilic organic UV filters from environmental water samples as model analytical application with excellent analytical features in terms of linearity, enrichment factors (67-791), limits of detection (low ng L -1 ), intra- and inter-day repeatability (RSD<15%) and relative recoveries (87-113%, 91-117% and 89-115% for river, sea and swimming pool water samples, respectively). Copyright © 2017 Elsevier B.V. All rights reserved.

  12. Carbon nanotube reinforced hollow fiber solid/liquid phase microextraction: a novel extraction technique for the measurement of caffeic acid in Echinacea purpurea herbal extracts combined with high-performance liquid chromatography.

    Science.gov (United States)

    Es'haghi, Zarrin; Golsefidi, Mazyar Ahmadi; Saify, Ali; Tanha, Ali Akbar; Rezaeifar, Zohre; Alian-Nezhadi, Zahra

    2010-04-23

    A new design of hollow fiber solid-liquid phase microextraction (HF-SLPME) was developed for the determination of caffeic acid in medicinal plants samples as Echinacea purpure. The membrane extraction with sorbent interface used in this research is a three-phase supported liquid membrane consisting of an aqueous (donor phase), organic solvent/nano sorbent (membrane) and aqueous (acceptor phase) system operated in direct immersion sampling mode. The multi-walled carbon nanotube dispersed in the organic solvent is held in the pores of a porous membrane supported by capillary forces and sonification. It is in contact with two aqueous phases: the donor phase, which is the aqueous sample, and the acceptor phase, usually an aqueous buffer. All microextraction experiments were supported using an Accurel Q3/2 polypropylene hollow fiber membrane (600 microm I.D., 200 microm wall thicknesses, and 0.2 microm pore size). The experimental setup is very simple and highly affordable. The hollow fiber is disposable, so single use of the fiber reduces the risk of cross-contamination and carry-over problems. The proposed method allows the very effective and enriched recuperation of an acidic analyte into one single extract. In order to obtain high enrichment and extraction efficiency of the analyte using this novel technique, the main parameters were optimized. Under the optimized extraction conditions, the method showed good linearity (0.0001-50 microg/L), repeatability, low limits of detection (0.00005 microg/L) and excellent enrichment (EF=2108). Copyright 2010 Elsevier B.V. All rights reserved.

  13. Coalescence of a Drop inside another Drop

    Science.gov (United States)

    Mugundhan, Vivek; Jian, Zhen; Yang, Fan; Li, Erqiang; Thoroddsen, Sigurdur

    2016-11-01

    Coalescence dynamics of a pendent drop sitting inside another drop, has been studied experimentally and in numerical simulations. Using an in-house fabricated composite micro-nozzle, a smaller salt-water drop is introduced inside a larger oil drop which is pendent in a tank containing the same liquid as the inner drop. On touching the surface of outer drop, the inner drop coalesces with the surrounding liquid forming a vortex ring, which grows in time to form a mushroom-like structure. The initial dynamics at the first bridge opening up is quantified using Particle Image Velocimetry (PIV), while matching the refractive index of the two liquids. The phenomenon is also numerically simulated using the open-source code Gerris. The problem is fully governed by two non-dimensional parameters: the Ohnesorge number and the diameter ratios of the two drops. The validated numerical model is used to better understand the dynamics of the phenomenon. In some cases a coalescence cascade is observed with liquid draining intermittently and the inner drop reducing in size.

  14. Determination of Plant Volatiles Using Solid Phase Microextraction GC-MS

    Science.gov (United States)

    Van Bramer, Scott; Goodrich, Katherine R.

    2015-01-01

    This experiment combines analytical techniques of solid phase microextraction and gas chromatography-mass spectrometry with easily relatable and accessible plant volatile chemistry (floral and vegetative scents of local/available plants). The biosynthesis and structure of these chemicals are of interest in the areas of organic chemistry,…

  15. Evaluation of the combination of a dispersive liquid-liquid microextraction method with micellar electrokinetic chromatography coupled to mass spectrometry for the determination of estrogenic compounds in milk and yogurt.

    Science.gov (United States)

    D'Orazio, Giovanni; Asensio-Ramos, María; Hernández-Borges, Javier; Rodríguez-Delgado, Miguel Ángel; Fanali, Salvatore

    2015-02-01

    In this work, the suitability of a methodology based on dispersive liquid-liquid microextraction (DLLME) has been evaluated for the extraction of four endoestrogens (estriol, 17α-estradiol, 17β-estradiol, and estrone), an exoestrogen (17α-etynylestradiol), and a mycotoxin (zearalenone), together with some of their major metabolites (2-methoxyestradiol, α-zearalanol, β-zearalanol, α-zearalenol, and β-zearalenol) from different types of milk (whole and skimmed cow milk and semiskimmed goat milk) and whole natural yogurt. The methodology includes a previous protein precipitation with acidified ACN and a defatting step with n-hexane. Separation of the analytes, determination, and quantification were developed by MEKC coupled to ESI-MS using a BGE containing an aqueous solution of ammonium perfluorooctanoate as MS friendly surfactant. Calibration, precision, and accuracy studies of the described DLLME-MEKC-MS/MS method were evaluated obtaining a good linearity and LODs in the low micrograms per liter range. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Trace determination of organophosphate esters in white wine, red wine, and beer samples using dispersive liquid-liquid microextraction combined with ultra-high-performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Pang, Long; Yang, Huiqiang; Yang, Peijie; Zhang, Hongzhong; Zhao, Jihong

    2017-08-15

    In this study, dispersive liquid-liquid microextraction coupled with ultra-high-performance liquid chromatography-tandem mass spectrometry was developed for the analysis of five representative organophosphate esters (OPEs) in wine samples. Under optimized conditions, the proposed method resulted in good linearity (R 2 >0.9933) over the range of 0.1-100μgL -1 , with limits of detection (LODs, S/N =3) and quantification (LOQs, S/N =10) in the ranges of 0.48-18.8ngL -1 and 1.58-62.5ngL -1 , respectively. Inter- and intra-assay precisions of RSD% ranged from 3.21% to 6.13% and from 1.69% to 7.63%, respectively. The spiked recoveries of target OPEs from white wine, red wine, and beer samples were in the ranges of 80-122%, 76-120%, and 76-110%, respectively, at two different concentration levels. The total concentrations of five OPEs found in white wine, red wine, and beer samples were in the ranges of 0.29-0.85μgL -1 , 1.00-3.05μgL -1 , and 0.86-1.47μgL -1 , respectively. Copyright © 2017 Elsevier Ltd. All rights reserved.

  17. Combination of microwave-assisted extraction and ultrasonic-assisted dispersive liquid-liquid microextraction for separation and enrichment of pyrethroids residues in Litchi fruit prior to HPLC determination.

    Science.gov (United States)

    Wang, Ke; Xie, Xiujuan; Zhang, Yi; Huang, Yuanxiang; Zhou, Shiyu; Zhang, Wei; Lin, Yuyang; Fan, Huajun

    2018-02-01

    A novel method for simultaneous determination of pyrethroids residues in Litchi fruit has been developed by HPLC-UV detection using microwave-assisted extraction (MAE) coupled with ultrasonic-assisted dispersive liquid-liquid microextraction (UADLLME). Extraction conditions of MAE and UADLLME were respectively investigated by single-factor experiments and response surface methodology. Optimized experimental conditions included 310μL of chlorobenzene as extraction solvent, 1.3mL of ethanol as dispersive solvent and 3min of extraction time for UADLLME. In the case of MAE, extraction temperature of 70°C, extraction time of 4min and solvent-to-materials ratio of 40:1 were adopted. Results demonstrated that the proposed method had good performance with linearity of 0.0050-4.98mg/L, recovery of 83.3-91.5%, RSDs below 5.6% and detection limit (LOD) of 1.15-2.46μg/L for six pyrethroids, offering higher extraction efficiency and larger enrichment factor. MAE-UADLLME provided a sensitive and efficient alternative to determination of trace amounts of pesticides residues in food samples. Copyright © 2017 Elsevier Ltd. All rights reserved.

  18. Combination of accelerated solvent extraction and vortex-assisted liquid-liquid microextraction for the determination of dimethyl fumarate in textiles and leathers by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Lu, Yang; Zhu, Yan

    2014-02-01

    A simple and environmentally friendly sample preparation procedure coupled with gas chromatography-mass spectrometry was developed to assay dimethyl fumarate in textiles and leathers. The sample preparation procedure involved an accelerated solvent extraction (ASE) using water as the extract solvent, followed by the extraction and concentration of dimethyl fumarate from the aqueous solution using vortex-assisted liquid-liquid microextraction (VALLME). The parameters affecting the ASE and VALLME were optimized to achieve the maximum extraction efficiency, and the performance of the developed method was evaluated. Good linearity was observed over the range assayed (0.01-1mg/kg) with a regression coefficient of 0.998. The limit of detection and enrichment factor for the VALLME step were 0.001 mg/kg and 53, respectively. The intra- and inter-day precision were below 8.9%, and the recovery was approximately 84-103%. The as-developed method was successfully applied to textiles and leather samples. © 2013 Elsevier B.V. All rights reserved.

  19. Determination of twelve herbicides in tobacco by a combination of solid–liquid–solid dispersive extraction using multi-walled carbon nanotubes, dispersive liquid-liquid micro-extraction, and detection by GC with triple quadrupole mass spectrometry

    International Nuclear Information System (INIS)

    Liao, Qie Gen; Zhou, Yao Min; Luo, Lin Guang; Wang, Li Bing; Feng, Xiao Hu

    2014-01-01

    We report on a method for the determination of twelve herbicides using solid–liquid–solid dispersive extraction (SLSDE), followed by dispersive liquid-liquid micro-extraction (DLLME) and quantitation by gas chromatography with triple quadrupole mass spectrometric detection. SLSDE was applied to the extraction of herbicides from tobacco samples using multi-walled carbon nanotubes (MWCNTs) as clean-up adsorbents. The effect of the quantity of MWCNTs on SLSDE, and of type and volume of extraction and disperser solvents and of salt effect on DLLME were optimized. Good linearity is obtained in the 5.0 - 500 μg kg −1 concentration range, with regression coefficients of >0.99. Intra-day and inter-day repeatability, expressed as relative standard deviations, are between 3 and 9 %. The recoveries in case of herbicide-spiked tobacco at concentration levels of 20.0, 50.0 and 100.0 g kg −1 ranged from 79 to 105 %, and LODs are between 1.5 and 6.1 μg kg −1 . All the tobacco samples were found to contain butralin and pendimethalin at levels ranging from 15.8 to 500.0 μg kg −1 . (author)

  20. Headspace sorptive solid phase microextraction (HS-SPME) combined with a spectrophotometry system: A simple glass devise for extraction and simultaneous determination of cyanide and thiocyanate in environmental and biological samples.

    Science.gov (United States)

    Al-Saidi, H M; Al-Harbi, Sami A; Aljuhani, E H; El-Shahawi, M S

    2016-10-01

    A simple, low cost and efficient headspace sorptive solid phase microextraction (HS-SPME) method for determination of cyanide has been developed. The system comprises of a glass tube with two valves and a moveable glass slide fixed at its centre. It includes an acceptor phase polyurethane foam treated mercury (II) dithizonate [Hg(HDz)2-PUF] complex fixed inside by a septum cap in a cylindrical configuration (5.0cm length and 1.0cm diameter). The extraction is based upon the contact of the acceptor phase to the headspace and subsequently measuring the absorbance of the recovered mercury (II) dithizonate from PUFs sorbent. Unlike other HSSE, extraction and back - extractions was carried out in a closed system, thereby improving the analytical performance by preventing the analyte loss. Under the optimized conditions, a linear calibration plot in the range of 1.0-50.0µmolL(-1) was achieved with limits of detection (LOD) and quantification (LOQ) of 0.34, 1.2µmolL(-1) CN(-), respectively. Simultaneous analysis of cyanide and thiocyanate in saliva was also performed with satisfactory recoveries. Copyright © 2016. Published by Elsevier B.V.

  1. Air-assisted Liquid Liquid Microextraction Combined with Graphite Furnace Atomic Absorption Spectrometry for Preconcentration and Determination of Trace Amount of Co(II and Ni(II Ions in Water Samples

    Directory of Open Access Journals (Sweden)

    Saeed Mohammad Sorouraddin

    2017-12-01

    Full Text Available A simple, rapid and efficient method has been developed for the extraction, preconcentration and determination of cobalt (II and nickel (II ions in water samples by air-assisted liquid-liquid microextraction (AALLME coupled with graphite furnace atomic absorption spectrometry (GFAAS. In the proposed method, much less volume of an organic solvent was used as the extraction solvent in the absence of disperser solvent. Fine organic droplets were formed by sucking and injecting of the mixture of aqueous sample solution and extraction solvent with a syringe for several times in a conical test tube. After extraction, phase separation was performed by centrifugation and the enriched analytes in the sedimented phase were determined by GFAAS. Several variables that could affect the extraction efficiency were investigated and optimized. Calibration graphs were linear in the range of 6.5-100 ng L-1. Detection limits for Co and Ni were 2.3 ng L-1 and 3 ng L-1, respectively. The accuracy of the developed procedure was checked by analyzing NRCC-SLRS4 Riverine water as a certified reference material. Finally, the proposed method has been successfully applied for the determination of cobalt (II and nickel (II ions in tap, surface and river water samples.

  2. Ionic liquid based vortex assisted liquid-liquid microextraction combined with liquid chromatography mass spectrometry for the determination of bisphenols in thermal papers with the aid of response surface methodology.

    Science.gov (United States)

    Asati, Ankita; Satyanarayana, G N V; Panchal, Smita; Thakur, Ravindra Singh; Ansari, Nasreen G; Patel, Devendra K

    2017-08-04

    A sensitive, rapid and efficient ionic liquid-based vortex assisted liquid-liquid microextraction (IL-VALLME) with Liquid Chromatography Mass spectrometry (LC-MS/MS) method is proposed for the determination of bisphenols in thermal paper. Extraction factors were systematically optimized by response surface methodology. Experimental factors showing significant effects on the analytical responses were evaluated using design of experiment. The limit of detection for Bisphenol-A (BPA) and Bisphenol-S (BPS) in thermal paper were 1.25 and 0.93μgkg -1 respectively. The dynamic linearity range for BPA was between 4 and 100μgkg -1 and the determination of coefficient (R 2 ) was 0.996. The values of the same parameters were 3-100μgkg -1 and 0.998 for BPS. The extraction recoveries of BPA and BPS in thermal paper were 101% and 99%. Percent relative standard deviation (% RSD) for matrix effect and matrix match effects were not more than 10%, for both bisphenols. The proposed method uses a statistical approach for the analysis of bisphenols in environmental samples, and is easy, rapid, requires minimum organic solvents and efficient. Copyright © 2017 Elsevier B.V. All rights reserved.

  3. Polypyrrole/montmorillonite nanocomposite as a new solid phase microextraction fiber combined with gas chromatography–corona discharge ion mobility spectrometry for the simultaneous determination of diazinon and fenthion organophosphorus pesticides

    International Nuclear Information System (INIS)

    Jafari, Mohammad T.; Saraji, Mohammad; Sherafatmand, Hossein

    2014-01-01

    Graphical abstract: - Highlights: • A novel SPME fiber based on polypyrrole/montmorillonite nanocomposites with highly porous and thermal stability was prepared. • The two-dimensional separation technique, GC–IMS, was used for analysis of complex matrices extracted by SPME. • Direct and simultaneous analysis of diazinon and fenthion in various real samples was successfully accomplished. - Abstract: A novel solid phase microextraction (SPME) fiber was prepared and coupled with gas chromatography corona discharge ion mobility spectrometry (GC–CD–IMS) based on polypyrrole/montmorillonite nanocomposites for the simultaneous determination of diazinon and fenthion. The nanocomposite polymer was coated using a three-electrode electrochemical system and directly deposited on a Ni–Cr wire by applying a constant potential. The scanning electron microscopy images revealed that the new fiber exhibited a rather porous and homogenous surface. The thermal stability of the fabricated fiber was investigated by thermogravimetric analysis. The effects of different parameters influencing the extraction efficiency such as extraction temperature and time, salt addition, stirring rate, the amount of nanoclay, and desorption temperature were investigated and optimized. The method was exhaustively evaluated in terms of sensitivity, recovery, and reproducibility. The linearity ranges of 0.05–10 and 0.08–10 μg L −1 , and the detection limits of 0.020 and 0.035 μg L −1 were obtained for diazinon and fenthion, respectively. The relative standard deviation values were calculated to be lower than 5% and 8% for intra-day and inter-day, respectively. Finally, the developed method was applied to determine the diazinon and fenthion (as model compounds) in cucumber, lettuce, apple, tap and river water samples. The satisfactory recoveries revealed the capability of the two-dimensional separation technique (retention time in GC and drift time in IMS) for the analysis of complex

  4. Ionic liquid-based dispersive liquid-liquid microextraction combined with high performance liquid chromatography-UV detection for simultaneous preconcentration and determination of Ni, Co, Cu and Zn in water samples

    Directory of Open Access Journals (Sweden)

    Asghari Alireza

    2014-01-01

    Full Text Available Ionic liquid-based dispersive liquid-liquid microextraction (IL-DLLME coupled with high performance liquid chromatography (HPLC-UV detection was developed for simultaneous extraction and determination of nickel, cobalt, copper and zinc ions. In the proposed approach, salophen (N,N'-bis(salisyliden-1,2-phenylenediamine was used as a chelating agent; the ionic liquid, 1-hexeyl-3-methylimidazolium hexafluorophosphate, and acetone were selected as extracting and dispersive solvents, respectively. After extraction, phase separation was performed by centrifugation and the sedimented phase (ionic liquid was solubilized in acetonitrile and directly injected into the HPLC for subsequent analysis. Baseline separation of metal ion complexes was achieved on a RP-C18 column using a gradient elution of the mixtures of methanol-acetonitrile-water as the mobile phase at a flow rate of 1.0 mL min-1. The influence of variables such as sample pH, concentration of the chelating agent, amount of ionic liquid (extraction solvent, disperser solvent volume, extraction time, salt effect and centrifugation speed were studied and optimized. Under the optimum conditions, the enrichment factor of 222 was obtained. The detection limits for Ni, Co, Cu and Zn were 0.8, 1.6, 1.9 and 2.8 μg L−1, respectively. The relative standard deviations (RSDs were in the range of 3.6-5.0 % for all of the investigated metal ions. The proposed procedure was successfully applied to the determination of the studied metal ions in water samples.

  5. Determination of brilliant green from fish pond water using carbon nanotube assisted pseudo-stir bar solid/liquid microextraction combined with UV-vis spectroscopy-diode array detection.

    Science.gov (United States)

    Es'haghi, Zarrin; Khooni, Maliheh Ahmadi-Kalateh; Heidari, Tahereh

    2011-08-01

    This paper describes the development of a new design of hollow fiber solid/liquid phase microextraction (HF-SLPME) for determination of brilliant green (BG) residues in water fish ponds. This method consists of an aqueous donor phase and carbon nanotube reinforced organic solvent (acceptor phase) operated in direct immersion sampling mode. The multi-walled carbon nanotube dispersed in the organic solvent is held in the pores and lumen of a porous polypropylene hollow fiber. It is in contact directly with the aqueous donor phase. In this method the solid/liquid extractor phase is supported using a polypropylene hollow fiber membrane. Both ends of the hollow fiber segment are sealed with magnetic stoppers. This device is placed inside the donor solution and plays the rule of a pseudo-stir bar. It is disposable, so single use of the fiber reduces the risk of carry-over problems. Brilliant green (BG) after extraction from the aqueous samples with mentioned HF-SLPME device was determined by ultraviolet-visible spectroscopy with diode array detection (UV-vis/DAD). The absorption wavelength was set to 625 nm (λ(max)). The effect of different variables on the extraction was evaluated and optimized to enhance the sensitivity and extraction efficiency of the proposed method. The calibration curve was linear in the range of 1.00-10,000 μg L(-1) of BG in the initial solution with R(2)=0.979. Detection limit, based on three times the standard deviation of the blank, was 0.55 μg L(-1). All experiments were carried out at room temperature (25±0.5°C). Copyright © 2011 Elsevier B.V. All rights reserved.

  6. Hollow fiber liquid-phase microextraction with in situ derivatization combined with gas chromatography-mass spectrometry for the determination of root exudate phenylamine compounds in hot pepper ( Capsicum annuum L.).

    Science.gov (United States)

    Sun, Haiyan; Wang, Yan

    2013-06-12

    Hollow fiber liquid-phase microextraction (HF-LPME) with derivatization was developed for the determination of three root exudate phenylamine compounds in hot pepper ( Capsicum annuum L.) by gas chromatography-mass spectrometry (GC-MS). The performance and applicability of the proposed procedure were evaluated through the extraction of 1-naphthylamine (1-NA), diphenylamine (DPA), and N-phenyl-2- naphthaleneamine (N-P-2-NA) in a recirculating hydroponic solution of hot pepper. Parameters affecting the extraction efficiency were investigated. The calibration curves showed a good linearity in the range of 0.1-10 μg mL(-1). The limits of detection (S/N = 3) for the three compounds were 0.096, 0.074, and 0.057 μg mL(-1), respectively. The enrichment factors reached 174, 196, and 230 at the concentration of 5 μg mL(-1), and relative standard deviations (RSD) of 9.5, 8.6, and 7.8% and 8.4, 7.6, and 6.2% were obtained at concentrations of 2 and 5 μg mL(-1) for 1-NA, DPA, and N-P-2-NA, respectively. Recoveries ranging from 90.2 to 96.1% and RSDs below 9.1% were obtained when HF-LPME with in situ derivatization was applied to determine root exudate 1-NA, DPA, and N-P-2-NA after 15 and 30 days of culture solution, respectively.

  7. Three-phase molecularly imprinted sol-gel based hollow fiber liquid-phase microextraction combined with liquid chromatography-tandem mass spectrometry for enrichment and selective determination of a tentative lung cancer biomarker.

    Science.gov (United States)

    Moein, Mohammad Mahdi; Javanbakht, Mehran; Karimi, Mohammad; Akbari-Adergani, Behrouz; Abdel-Rehim, Mohamed

    2015-07-15

    In the present study, the modification of a polysulfone hollow fiber membrane with in situ molecularly imprinted sol-gel process (as a novel and one-step method) was prepared and investigated. 3-(propylmethacrylate)trimethoxysilane (3PMTMOS) as an inorganic precursor was used for preparation of molecularly imprinted sol-gel. The modified molecularly imprinted sol-gel hollow fiber membrane (MSHM) was used for the liquid-phase microextraction (LPME) of hippuric acid (HA) in human plasma and urine samples. MSHM as a selective, robust, and durable tool was used for at least 50 extractions without significant decrease in the extraction efficiency. The non-molecularly imprinted sol-gel hollow fiber membrane (NSHM) as blank hollow fiber membrane was prepared by the same process, only without HA. To achieve the best condition, influential parameters on the extraction efficiency were thoroughly investigated. The capability of this robust, green, and simple method for extraction of HA was successfully accomplished with LC/MS/MS. The limits of detection (LOD) and quantification (LOQ) in human plasma and urine samples were 0.3 and 1.0nmolL(-1), respectively. The standard calibration curves were obtained within the concentration range 1-2000nmolL(-1) for HA in human plasma and urine. The coefficients of determination (r(2)) were ≥0.998. The obtained data exhibited recoveries were higher than 89% for the extraction of HA in human plasma and urine samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  8. Scanning drop sensor

    Science.gov (United States)

    Jin, Jian; Xiang, Chengxiang; Gregoire, John M.; Shinde, Aniketa A.; Guevarra, Dan W.; Jones, Ryan J.; Marcin, Martin R.; Mitrovic, Slobodan

    2017-05-09

    Electrochemical or electrochemical and photochemical experiments are performed on a collection of samples by suspending a drop of electrolyte solution between an electrochemical experiment probe and one of the samples that serves as a test sample. During the electrochemical experiment, the electrolyte solution is added to the drop and an output solution is removed from the drop. The probe and collection of samples can be moved relative to one another so the probe can be scanned across the samples.

  9. Bubble and drop interfaces

    CERN Document Server

    Miller

    2011-01-01

    The book aims at describing the most important experimental methods for characterizing liquid interfaces, such as drop profile analysis, bubble pressure and drop volume tensiometry, capillary pressure technique, and oscillating drops and bubbles. Besides the details of experimental set ups, also the underlying theoretical basis is presented in detail. In addition, a number of applications based on drops and bubbles is discussed, such as rising bubbles and the very complex process of flotation. Also wetting, characterized by the dynamics of advancing contact angles is discussed critically. Spec

  10. Improvement of solid-phase microextraction efficiency by the application of a carbon-nanotubes-based ternary microextraction fiber composite.

    Science.gov (United States)

    Mohammadiazar, Sirwan; Fallahpour, Nastaran; Roostaie, Ali; Ebrahimi, Bahram

    2017-09-01

    In this study, a novel technique is proposed for preparation of an efficient and unbreakable metal-wire-supported solid-phase microextraction fiber. A sol-gel film was deposited on electrophoretically deposited carbon nanotubes on a stainless-steel wire. The applicability of the fiber was evaluated through the extraction of some aromatic pollutants as model compounds from the headspace of aqueous samples in combination with gas chromatography and mass spectrometry. The parameters affecting the structure and extraction efficiency of the fiber (including the type of solvent, time, and potential for electrophoretic deposition) and the parameters affecting the extraction efficiency (such as coating type, salt content, extraction temperature, and time) were investigated. The results showed that the film thickness will be increased by increasing the potential and time duration. Finally, the characterization of the deposited film was accomplished by scanning electron microscopy and thermogravimetric analysis. After the optimization of the extraction parameters, the limit of detection of less than 20 pg/mL was achieved, and the calibration curves were all linear (r 2  ≥ 0.9737), in the range from 50 to 500 pg/mL. The solid-phase microextraction fiber has a high mechanical strength; good stability and long service life, making it potentially applicable in the extraction of trace polycyclic aromatic hydrocarbons from aqueous samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. A sensitive microextraction by packed sorbent-based methodology combined with ultra-high pressure liquid chromatography as a powerful technique for analysis of biologically active flavonols in wines.

    Science.gov (United States)

    Silva, Catarina L; Gonçalves, João L; Câmara, José S

    2012-08-20

    A new approach based on microextraction by packed sorbent (MEPS) and reversed-phase high-throughput ultra high pressure liquid chromatography (UHPLC) method that uses a gradient elution and diode array detection to quantitate three biologically active flavonols in wines, myricetin, quercetin, and kaempferol, is described. In addition to performing routine experiments to establish the validity of the assay to internationally accepted criteria (selectivity, linearity, sensitivity, precision, accuracy), experiments are included to assess the effect of the important experimental parameters such as the type of sorbent material (C2, C8, C18, SIL, and C8/SCX), number of extraction cycles (extract-discard), elution volume, sample volume, and ethanol content, on the MEPS performance. The optimal conditions of MEPS extraction were obtained using C8 sorbent and small sample volumes (250μL) in five extraction cycle and in a short time period (about 5min for the entire sample preparation step). Under optimized conditions, excellent linearity (R(values)(2)>0.9963), limits of detection of 0.006μgmL(-1) (quercetin) to 0.013μgmL(-1) (myricetin) and precision within 0.5-3.1% were observed for the target flavonols. The average recoveries of myricetin, quercetin and kaempferol for real samples were 83.0-97.7% with relative standard deviation (RSD, %) lower than 1.6%. The results obtained showed that the most abundant flavonol in the analyzed samples was myricetin (5.8±3.7μgmL(-1)). Quercetin (0.97±0.41μgmL(-1)) and kaempferol (0.66±0.24μgmL(-1)) were found in a lower concentration. The optimized MEPS(C8) method was compared with a reverse-phase solid-phase extraction (SPE) procedure using as sorbent a macroporous copolymer made from a balanced ratio of two monomers, the lipophilic divinylbenzene and the hydrophilic N-vinylpyrrolidone (Oasis HLB) were used as reference. MEPS(C8) approach offers an attractive alternative for analysis of flavonols in wines, providing a number of

  12. Development and validation of a fast ionic liquid-based dispersive liquid-liquid microextraction procedure combined with LC-MS/MS analysis for the quantification of benzodiazepines and benzodiazepine-like hypnotics in whole blood.

    Science.gov (United States)

    De Boeck, Marieke; Missotten, Sophie; Dehaen, Wim; Tytgat, Jan; Cuypers, Eva

    2017-05-01

    To date, thorough clean-up of complex biological samples remains an essential part of the analytical process. The solid phase extraction (SPE) technique is the well-known standard, however, its main weaknesses are the labor-intensive and time-consuming protocols. In this respect, dispersive liquid-liquid microextractions (DLLME) seem to offer less complex and more efficient extraction procedures. Furthermore, ionic liquids (ILs) - liquid salts - are emerging as new promising extraction solvents, thanks to their non-flammable nature, negligible vapor pressure and easily adaptable physiochemical properties. In this study, we investigated whether ILs can be used as an extraction solvent in a DLLME procedure for the extraction of a broad range of benzodiazepines and benzodiazepine-like hypnotics in whole blood samples. 1.0mL whole blood was extracted using an optimized 30-min IL-based DLLME procedure, followed by LC-ESI(+)-MS/MS analysis in scheduled MRM scan mode. The optimized analytical method was successfully validated for 7-aminoflunitrazepam, alprazolam, bromazepam, clobazam, clonazepam, clotiazepam, diazepam, estazolam, ethyl loflazepate, etizolam, flurazepam, lormetazepam, midazolam, oxazepam, prazepam, temazepam, triazolam, zolpidem and zopiclone. The method showed good selectivity for endogenous interferences based on 12 sources of blank whole blood. No benzodiazepine interferences were observed, except for clorazepate and nordiazepam, which were excluded from the quantitative method. Matrix-matched calibration curves were constructed covering the whole therapeutic range, including low toxic plasma concentrations. Accuracy and precision results met the proposed acceptance criteria for the vast majority of compounds, except for brotizolam, chlordiazepoxide, cloxazolam, flunitrazepam, loprazolam, lorazepam and nitrazepam, which can only be determined in a semi-quantitative way. Recoveries were within the range of 24.7%-127.2% and matrix effects were within 20

  13. Low-density solvent-based vortex-assisted surfactant-enhanced-emulsification liquid-liquid microextraction combined with gas chromatography-mass spectrometry for the fast determination of phthalate esters in bottled water.

    Science.gov (United States)

    Zhang, Yufeng; Lee, Hian Kee

    2013-01-25

    For the first time, a novel low-density solvent-based vortex-assisted surfactant-enhanced-emulsification liquid-liquid microextraction (LDS-VSLLME) was developed for the fast, simple and efficient determination of six phthalate esters (PEs) in bottled water samples followed by gas chromatography-mass spectrometry (GC-MS). In the extraction procedure, the aqueous sample solution was injected into a mixture of extraction solvent (toluene) and surfactant (cetyltrimethyl ammonium bromide), which were placed in a glass tube with conical bottom, to form an emulsion by the assistance of vortex agitation. After extraction and phase separation by centrifugation, and removal of the spent sample, the toluene extract was collected and analyzed by GC-MS. The addition of surfactant enhanced the dispersion of extraction solvent in aqueous sample and was also favorable for the mass transfer of the analytes from the aqueous sample to the extraction solvent. Moreover, using a relatively less toxic surfactant as the emulsifier agent overcame the disadvantages of traditional organic dispersive solvents that are usually highly toxic and expensive and might conceivably decrease extraction efficiency to some extent since they are not as effective as surfactants themselves in generating an emulsion. With the aid of surfactant and vortex agitation to achieve good organic extraction solvent dispersion, extraction equilibrium was achieved within 1 min, indicating it was a fast sample preparation technique. Another prominent feature of the method was the simple procedure to collect a less dense than water solvent by a microsyringe. After extraction and phase separation, the aqueous sample was removed using a 5-mL syringe, thus leaving behind the extract, which was retrieved easily. This novel method simplifies the use of low-density solvents in DLLME. Under the optimized conditions, the proposed method provided good linearity in the range of 0.05-25 μg/L, low limits of detection (8-25 ng

  14. Turbulence, bubbles and drops

    NARCIS (Netherlands)

    van der Veen, Roeland

    2016-01-01

    In this thesis, several questions related to drop impact and Taylor-Couette turbulence are answered. The deformation of a drop just before impact can cause a bubble to be entrapped. For many applications, such as inkjet printing, it is crucial to control the size of this entrapped bubble. To study

  15. Application of head-space solid-phase microextraction for the analysis of volatile metabolites emitted by Penicillium species

    DEFF Research Database (Denmark)

    Nilsson, Torben; Larsen, Thomas Ostenfeld; Montanarella, Luca

    1996-01-01

    Head-space solid-phase microextraction (HS-SPME) has been used to collect volatile organic compounds (VOCs) emitted from fungi of the genus Penicillium. Gas chromatography combined with mass spectrometry (GC-MS) was employed for the analysis of the profiles of volatile metabolites characteristic ......-SPME has a great potential use in the analysis of biogenic VOC emissions, including chemotaxonomical studies....

  16. Drop Tower Physics

    Science.gov (United States)

    Dittrich, William A. Toby

    2014-10-01

    The drop towers of yesteryear were used to make lead shot for muskets, as described in The Physics Teacher1 in April 2012. However, modern drop towers are essentially elevators designed so that the cable can "break" on demand, creating an environment with microgravity for a short period of time, currently up to nine seconds at the drop tower in Bremen, Germany. Using these drop towers, one can briefly investigate various physical systems operating in this near zero-g environment. The resulting "Drop Tower Physics" is a new and exciting way to challenge students with a physical example that requires solid knowledge of many basic physics principles, and it forces them to practice the scientific method. The question is, "How would a simple toy, like a pendulum, behave when it is suddenly exposed to a zero-g environment?" The student must then postulate a particular behavior, test the hypothesis against physical principles, and if the hypothesis conforms to these chosen physical laws, the student can formulate a final conclusion. At that point having access to a drop tower is very convenient, in that the student can then experimentally test his or her conclusion. The purpose of this discussion is to explain the response of these physical systems ("toys") when the transition is made to a zero-g environment and to provide video demonstrations of this behavior to support in-class discussions of Drop Tower Physics.

  17. Magnetic in-tube solid phase microextraction.

    Science.gov (United States)

    Moliner-Martínez, Y; Prima-Garcia, Helena; Ribera, Antonio; Coronado, Eugenio; Campíns-Falcó, P

    2012-08-21

    We report a new in-tube solid phase microextraction approach named magnetic in-tube solid phase microextraction, magnetic-IT-SPME. Magnetic-IT-SPME has been developed, taking advantage of magnetic microfluidic principles with the aim to improve extraction efficiency of IT-SPME systems. First, a magnetic hybrid material formed by Fe(3)O(4) nanoparticles supported on SiO(2) was synthesized and immobilized in the surface of a bared fused silica capillary column to obtain a magnetic adsorbent extraction phase. The capillary column was placed inside a magnetic coil that allowed the application of a variable magnetic field. Acetylsalicylic acid, acetaminophen, atenolol, diclofenac, and ibuprofen were tested as target analytes. The application of a controlled magnetic field resulted in quantitative extraction efficiencies of the target analytes between 70 and 100%. These results demonstrated that magnetic forces solve the low extraction efficiency (10-30%) of IT-SPME systems, which is one of their main drawbacks.

  18. Preparation and Stability of Voriconazole Eye Drop Solution▿

    OpenAIRE

    Dupuis, Antoine; Tournier, Nicolas; Le Moal, Gwenaël; Venisse, Nicolas

    2008-01-01

    The combined systemic and topical administration of voriconazole has successfully been used to treat keratomycosis. Because no voriconazole eye drop product is commercially available, we prepared a sterile eye drop solution (10 mg/ml). Voriconazole remains stable over 30 days, providing an eye drop solution suitable for use for the topical treatment of fungal keratitis.

  19. Steam distillation-solid-phase microextraction for the detection of Ephedra sinica in herbal preparations.

    Science.gov (United States)

    Tellez, Mari R; Khan, Ikhlas A; Schaneberg, Brian T; Crockett, Sara L; Rimando, Agnes M; Kobaisy, Mozaina

    2004-01-30

    A new method involving concurrent solid-phase microextraction combined with continuous hydrodistillation of essential oil was developed. This new methodology allowed for the detection by GC-MS of very small amounts of a diagnostic peak for the authentication of Ephedra sinica, in a short period of time and using only small sample sizes. This diagnostic peak was identified as 4-vinylanisole, and elucidated from the chromatographic profile allowed for the identification of a sample as E. sinica among other species investigated in this study. To the best of our knowledge this is the first report on using continuous solid-phase microextraction coupled to hydrodistillation for the investigation of essential oil components, and the first report of 4-vinylanisole as a marker compound for E. sinica. A total of 46 collections representing 21 species of Ephedra were studied.

  20. Impact of granular drops

    KAUST Repository

    Marston, J. O.

    2013-07-15

    We investigate the spreading and splashing of granular drops during impact with a solid target. The granular drops are formed from roughly spherical balls of sand mixed with water, which is used as a binder to hold the ball together during free-fall. We measure the instantaneous spread diameter for different impact speeds and find that the normalized spread diameter d/D grows as (tV/D)1/2. The speeds of the grains ejected during the “splash” are measured and they rarely exceed twice that of the impact speed.

  1. Drop impact splashing and air entrapment

    KAUST Repository

    Thoraval, Marie-Jean

    2013-03-01

    Drop impact is a canonical problem in fluid mechanics, with numerous applications in industrial as well as natural phenomena. The extremely simple initial configuration of the experiment can produce a very large variety of fast and complex dynamics. Scientific progress was made in parallel with major improvements in imaging and computational technologies. Most recently, high-speed imaging video cameras have opened the exploration of new phenomena occurring at the micro-second scale, and parallel computing allowed realistic direct numerical simulations of drop impacts. We combine these tools to bring a new understanding of two fundamental aspects of drop impacts: splashing and air entrapment. The early dynamics of a drop impacting on a liquid pool at high velocity produces an ejecta sheet, emerging horizontally in the neck between the drop and the pool. We show how the interaction of this thin liquid sheet with the air, the drop or the pool, can produce micro-droplets and bubble rings. Then we detail how the breakup of the air film stretched between the drop and the pool for lower impact velocities can produce a myriad of micro-bubbles.

  2. Switchable polarity solvent for liquid phase microextraction of Cd(II) as pyrrolidinedithiocarbamate chelates from environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Yilmaz, Erkan, E-mail: kimyager_erkan@hotmail.com; Soylak, Mustafa, E-mail: soylak@erciyes.edu.tr

    2015-07-30

    A switchable polarity solvent was synthesized from triethylamine (TEA)/water/CO{sub 2} (Dry ice) via proton transfer reaction has been used for the microextraction of cadmium(II) as pyrrolidinedithiocarbamate (APDC) chelate. Cd(II)-APDC chelate was extracted into the switchable polarity solvent drops by adding 2 mL 10 M sodium hydroxide solution. Analytical parameters affecting the complex formation and microextraction efficiency such as pH, amount of ligand, volume of switchable polarity solvent and NaOH, sample volume were optimized. The effects of foreign ions were found tolerably. Under optimum conditions, the detection limit was 0.16 μg L{sup −1} (3Sb/m, n = 7) and the relative standard deviation was 5.4% (n = 7). The method was validated by the analysis of certified reference materials (TMDA-51.3 fortified water, TMDA-53.3 fortified water and SPS-WW2 waste water, 1573a Tomato Leaves and Oriental Basma Tobacco Leaves (INCT-OBTL-5)) and addition/recovery tests. The method was successfully applied to determination of cadmium contents of water, vegetable, fruit and cigarette samples. - Highlights: • Switchable polarity solvent was synthesized from triethylamine (TEA)/water/CO{sub 2}. • The switchable polarity solvent has been used for the microextraction of cadmium(II). • The important factors were optimized. • The method was applied to determination of cadmium in real samples.

  3. Large drops cause complete coalescence

    Indian Academy of Sciences (India)

    The thin film below the drop drains out slowly with time, finally creating a hole in the drop when it comes in contact with the interface at t=0.37 Tc, a small matrix drop, also called satellite drop, is seen to be trapped during the film rupture. Such an entrapment was observed by Thoroddsen et al (2008) and Chen et al (2006).

  4. Two secondary drops

    Indian Academy of Sciences (India)

    Figure shows formation of two secondary drops of unequal size and their merger. The process is same as the earlier process until t= 0.039 Tc with necking occurring at two places, one at the bottom of the column and the other at the middle. The necking at the middle of the liquid column is due to Raleigh instability.

  5. Two secondary drops

    Indian Academy of Sciences (India)

    First page Back Continue Last page Overview Graphics. Notes: Figure shows formation of two secondary drops of unequal size and their merger. The process is same as the earlier process until t= 0.039 Tc with necking occurring at two places, one at the bottom of the column and the other at the middle. The necking at the ...

  6. Lambda-dropping

    DEFF Research Database (Denmark)

    Danvy, Olivier; Schultz, Ulrik Pagh

    1997-01-01

    the parameters that any of their callees might possibly need. Both lambda-lifting and lambda-dropping thus require one to compute a transitive closure over the call graph:• for lambda-lifting: to establish the Def/Use path of each free variable (these free variables are then added as parameters to each......Lambda-lifting a functional program transforms it into a set of recursive equations. We present the symmetric transformation: lambda-dropping. Lambda-dropping a set of recursive equations restores block structure and lexical scope.For lack of scope, recursive equations must carry around all...... of the functions in the call path);• for lambda-dropping: to establish the Def/Use path of each parameter (parameters whose use occurs in the same scope as their definition do not need to be passed along in the call path).Without free variables, a program is scope-insensitive. Its blocks are then free...

  7. Operator care and eco-concerned development of a fast, facile and economical assay for basic nitrogenous drugs based on simplified ion-pair mini-scale extraction using safer solvent combined with drop-based spectrophotometry.

    Science.gov (United States)

    Plianwong, Samarwadee; Sripattanaporn, Areerut; Waewsa-nga, Kwanrutai; Buacheen, Parin; Opanasopit, Praneet; Ngawhirunpat, Tanasait; Rojanarata, Theerasak

    2012-08-30

    A fast, facile, and economical assay for basic nitrogenous drugs has been developed based on the mini-scale extraction of the drug-dye ion pair complex combined with the use of safe-for-analyst and eco-friendlier organic extractant and drop-based micro-spectrophotometry. Instead of using large volume devices, the extraction was simply carried out in typical 1.5 mL microcentrifuge tubes along with the use of micropipettes for accurate transfer of liquids, vortex mixer for efficient partitioning of solutes and benchtop centrifuge for rapid phase separation. In the last step, back-extraction was performed by using the microvolume of acidic solution in order to concentrate the colored species into a confined aqueous microdrop and to keep the analyst away from unwanted contact and inhalation of organic solvents during the quantitation step which was achieved by using cuvetteless UV-vis micro-spectrophotometry without any prior dilutions. Using chlorpheniramine maleate as a representative analyte and n-butyl acetate as a less toxic and non-ozone depleting extractant, the miniaturized method was less laborious and much faster. It was accurate, precise and insensitive to the interferences from common excipients. Notably, it gave the assay results of drug in tablets and oral solution comparable to the large-scale pharmacopeial method while the consumption of organic solvents and the release of wastes were lowered by 200-400 folds. Copyright © 2012 Elsevier B.V. All rights reserved.

  8. Novel approach to high-throughput determination of endocrine disruptors using recycled diatomaceous earth as a green sorbent phase for thin-film solid-phase microextraction combined with 96-well plate system.

    Science.gov (United States)

    Kirschner, Nicolas; Dias, Adriana Neves; Budziak, Dilma; da Silveira, Cristian Berto; Merib, Josias; Carasek, Eduardo

    2017-12-15

    A sustainable approach to TF-SPME is presented using recycled diatomaceous earth, obtained from a beer purification process, as a green sorbent phase for the determination of bisphenol A (BPA), benzophenone (BzP), triclocarban (TCC), 4-methylbenzylidene camphor (4-MBC) and 2-ethylhexyl-p-methoxycinnamate (EHMC) in environmental water samples. TF-SPME was combined with a 96-well plate system allowing for high-throughput analysis due to the simultaneous extraction/desorption up to 96 samples. The proposed sorbent phase exhibited good stability in organic solvents, as well as satisfactory analytical performance. The optimized method consisted of 240 min of extraction at pH 6 with the addition of NaCl (15% w/v). A mixture of MeOH:ACN (50:50 v/v) was used for the desorption the analytes, using a time of 30 min. Limits of detection varied from 1 μg L -1 for BzP and TCC to 8 μg L -1 for the other analytes, and R 2 ranged from 0.9926 for 4-MBC to 0.9988 for BPA. This novel and straightforward approach offers an environmentally-friendly and very promising alternative for routine analysis. . The total sample preparation time per sample was approximately 2.8 min, which is a significant advantage when a large number of analytical run is required. Copyright © 2017 Elsevier B.V. All rights reserved.

  9. Applications of Experimental Design to the Optimization of Microextraction Sample Preparation Parameters for the Analysis of Pesticide Residues in Fruits and Vegetables.

    Science.gov (United States)

    Abdulra'uf, Lukman Bola; Sirhan, Ala Yahya; Tan, Guan Huat

    2015-01-01

    Sample preparation has been identified as the most important step in analytical chemistry and has been tagged as the bottleneck of analytical methodology. The current trend is aimed at developing cost-effective, miniaturized, simplified, and environmentally friendly sample preparation techniques. The fundamentals and applications of multivariate statistical techniques for the optimization of microextraction sample preparation and chromatographic analysis of pesticide residues are described in this review. The use of Placket-Burman, Doehlert matrix, and Box-Behnken designs are discussed. As observed in this review, a number of analytical chemists have combined chemometrics and microextraction techniques, which has helped to streamline sample preparation and improve sample throughput.

  10. Headspace Solid-Phase Microextraction Coupled with Gas ...

    African Journals Online (AJOL)

    contact temperature measurement system (ONTMS). Headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC-MS) was used to analyze the volatile composition of raw FCP and its various ...

  11. Head-Space Solid Phase Micro-extraction Followed by GC/MS Analysis of the Volatile Components in Seeds of Cinnamonum camphora

    OpenAIRE

    Yang Yong; Tao Wenyi

    2005-01-01

    The volatile components in seeds of Cinnamomum camphora were analyzed by Solid Phase Micro-extraction (SPME) combined with GC/MS. Twenty four main kinds of volatile compounds, among which the Sesquiterpene (29%), 3-Hexen-2-one (25%) and Monoterpene (10.22%), were separated and analyzed.

  12. Negligible depletion solid-phase microextraction with radiolabeled analytes to study free concentrations and protein binding : an example with [3H]Estradiol

    NARCIS (Netherlands)

    Heringa, M.B.; Pastor, D.; Algra, J.; Vaes, W.H.J.; Hemmens, J.L.M.

    2002-01-01

    A new method is presented that enables sensitive measurement of free concentrations of radiolabeled ligands. Additionally, protein binding of radiochemicals in complex matrixes can be determined with this new technique that combines negligible depletion solid-phase microextraction (nd-SPME) with

  13. Simultaneous derivatization and extraction of primary amines in river water with dynamic hollow fiber liquid-phase microextraction followed by gas chromatography-mass spectrometric detection.

    Science.gov (United States)

    Chia, Kan-Jung; Huang, Shang-Da

    2006-01-20

    A one-step derivatization and extraction technique for the determination of primary amines in river water by liquid-phase microextraction (LPME) is presented. In this method the primary amines are derivatized with pentafluorobenzaldehyde (PFBAY) in aqueous solution and extracted by dynamic hollow fiber-protected-LPME (HF-LPME) simultaneously. The effects of solvent selection, sample agitation, extraction time, extraction temperature and salt concentration on the extraction performance are investigated. High enrichments (172-244-fold) and good repeatabilities (RSD less than 7.2%) were obtained. Linearity in this developed method was ranging from 1 to 500 ng/ml, and the correlation coefficients (R2) were between 0.992 and 0.998. Comparisons of sensitivity and precision between dynamic HF-LPME and single-drop liquid-phase microextraction (SDME) were also made.

  14. Lifetime of oil drops pressed by buoyancy against a planar interface: Large drops

    Science.gov (United States)

    Rojas, Clara; García-Sucre, Máximo; Urbina-Villalba, Germán

    2010-11-01

    In a previous report [C. Rojas, G. Urbina-Villalba, and M. García-Sucre, Phys. Rev. E 81, 016302 (2010)10.1103/PhysRevE.81.016302] it was shown that emulsion stability simulations are able to reproduce the lifetime of micrometer-size drops of hexadecane pressed by buoyancy against a planar water-hexadecane interface. It was confirmed that small drops (ri<10μm) stabilized with β -casein behave as nondeformable particles, moving with a combination of Stokes and Taylor tensors as they approach the interface. Here, a similar methodology is used to parametrize the potential of interaction of drops of soybean oil stabilized with bovine serum albumin. The potential obtained is then employed to study the lifetime of deformable drops in the range 10≤ri≤1000μm . It is established that the average lifetime of these drops can be adequately replicated using the model of truncated spheres. However, the results depend sensibly on the expressions of the initial distance of deformation and the maximum film radius used in the calculations. The set of equations adequate for large drops is not satisfactory for medium-size drops (10≤ri≤100μm) , and vice versa. In the case of large particles, the increase in the interfacial area as a consequence of the deformation of the drops generates a very large repulsive barrier which opposes coalescence. Nevertheless, the buoyancy force prevails. As a consequence, it is the hydrodynamic tensor of the drops which determine the characteristic behavior of the lifetime as a function of the particle size. While the average values of the coalescence time of the drops can be justified by the mechanism of film thinning, the scattering of the experimental data of large drops cannot be rationalized using the methodology previously described. A possible explanation of this phenomenon required elaborate simulations which combine deformable drops, capillary waves, repulsive interaction forces, and a time-dependent surfactant adsorption.

  15. Solid-phase microextraction and the human fecal VOC metabolome.

    Directory of Open Access Journals (Sweden)

    Emma Dixon

    2011-04-01

    Full Text Available The diagnostic potential and health implications of volatile organic compounds (VOCs present in human feces has begun to receive considerable attention. Headspace solid-phase microextraction (SPME has greatly facilitated the isolation and analysis of VOCs from human feces. Pioneering human fecal VOC metabolomic investigations have utilized a single SPME fiber type for analyte extraction and analysis. However, we hypothesized that the multifarious nature of metabolites present in human feces dictates the use of several diverse SPME fiber coatings for more comprehensive metabolomic coverage. We report here an evaluation of eight different commercially available SPME fibers, in combination with both GC-MS and GC-FID, and identify the 50/30 µm CAR-DVB-PDMS, 85 µm CAR-PDMS, 65 µm DVB-PDMS, 7 µm PDMS, and 60 µm PEG SPME fibers as a minimal set of fibers appropriate for human fecal VOC metabolomics, collectively isolating approximately 90% of the total metabolites obtained when using all eight fibers. We also evaluate the effect of extraction duration on metabolite isolation and illustrate that ex vivo enteric microbial fermentation has no effect on metabolite composition during prolonged extractions if the SPME is performed as described herein.

  16. First drop dissimilarity in drop-on-demand inkjet devices

    International Nuclear Information System (INIS)

    Famili, Amin; Palkar, Saurabh A.; Baldy, William J. Jr.

    2011-01-01

    As inkjet printing technology is increasingly applied in a broader array of applications, careful characterization of its method of use is critical due to its inherent sensitivity. A common operational mode in inkjet technology known as drop-on-demand ejection is used as a way to deliver a controlled quantity of material to a precise location on a target. This method of operation allows ejection of individual or a sequence (burst) of drops based on a timed trigger event. This work presents an examination of sequences of drops as they are ejected, indicating a number of phenomena that must be considered when designing a drop-on-demand inkjet system. These phenomena appear to be driven by differences between the first ejected drop in a burst and those that follow it and result in a break-down of the linear relationship expected between driving amplitude and drop mass. This first drop, as quantified by high-speed videography and subsequent image analysis, can be different in morphology, trajectory, velocity, and volume from subsequent drops within a burst. These findings were confirmed orthogonally by both volume and mass measurement techniques which allowed quantitation down to single drops.

  17. Recent Trends in Microextraction Techniques Employed in Analytical and Bioanalytical Sample Preparation

    Directory of Open Access Journals (Sweden)

    Abuzar Kabir

    2017-12-01

    Full Text Available Sample preparation has been recognized as a major step in the chemical analysis workflow. As such, substantial efforts have been made in recent years to simplify the overall sample preparation process. Major focusses of these efforts have included miniaturization of the extraction device; minimizing/eliminating toxic and hazardous organic solvent consumption; eliminating sample pre-treatment and post-treatment steps; reducing the sample volume requirement; reducing extraction equilibrium time, maximizing extraction efficiency etc. All these improved attributes are congruent with the Green Analytical Chemistry (GAC principles. Classical sample preparation techniques such as solid phase extraction (SPE and liquid-liquid extraction (LLE are being rapidly replaced with emerging miniaturized and environmentally friendly techniques such as Solid Phase Micro Extraction (SPME, Stir bar Sorptive Extraction (SBSE, Micro Extraction by Packed Sorbent (MEPS, Fabric Phase Sorptive Extraction (FPSE, and Dispersive Liquid-Liquid Micro Extraction (DLLME. In addition to the development of many new generic extraction sorbents in recent years, a large number of molecularly imprinted polymers (MIPs created using different template molecules have also enriched the large cache of microextraction sorbents. Application of nanoparticles as high-performance extraction sorbents has undoubtedly elevated the extraction efficiency and method sensitivity of modern chromatographic analyses to a new level. Combining magnetic nanoparticles with many microextraction sorbents has opened up new possibilities to extract target analytes from sample matrices containing high volumes of matrix interferents. The aim of the current review is to critically audit the progress of microextraction techniques in recent years, which has indisputably transformed the analytical chemistry practices, from biological and therapeutic drug monitoring to the environmental field; from foods to phyto

  18. Extensible automated dispersive liquid–liquid microextraction

    Energy Technology Data Exchange (ETDEWEB)

    Li, Songqing; Hu, Lu; Chen, Ketao; Gao, Haixiang, E-mail: hxgao@cau.edu.cn

    2015-05-04

    Highlights: • An extensible automated dispersive liquid–liquid microextraction was developed. • A fully automatic SPE workstation with a modified operation program was used. • Ionic liquid-based in situ DLLME was used as model method. • SPE columns packed with nonwoven polypropylene fiber was used for phase separation. • The approach was applied to the determination of benzoylurea insecticides in water. - Abstract: In this study, a convenient and extensible automated ionic liquid-based in situ dispersive liquid–liquid microextraction (automated IL-based in situ DLLME) was developed. 1-Octyl-3-methylimidazolium bis[(trifluoromethane)sulfonyl]imide ([C{sub 8}MIM]NTf{sub 2}) is formed through the reaction between [C{sub 8}MIM]Cl and lithium bis[(trifluoromethane)sulfonyl]imide (LiNTf{sub 2}) to extract the analytes. Using a fully automatic SPE workstation, special SPE columns packed with nonwoven polypropylene (NWPP) fiber, and a modified operation program, the procedures of the IL-based in situ DLLME, including the collection of a water sample, injection of an ion exchange solvent, phase separation of the emulsified solution, elution of the retained extraction phase, and collection of the eluent into vials, can be performed automatically. The developed approach, coupled with high-performance liquid chromatography–diode array detection (HPLC–DAD), was successfully applied to the detection and concentration determination of benzoylurea (BU) insecticides in water samples. Parameters affecting the extraction performance were investigated and optimized. Under the optimized conditions, the proposed method achieved extraction recoveries of 80% to 89% for water samples. The limits of detection (LODs) of the method were in the range of 0.16–0.45 ng mL{sup −1}. The intra-column and inter-column relative standard deviations (RSDs) were <8.6%. Good linearity (r > 0.9986) was obtained over the calibration range from 2 to 500 ng mL{sup −1}. The proposed

  19. Recent Microextraction Techniques for Determination and Chemical Speciation of Selenium

    Directory of Open Access Journals (Sweden)

    Ibrahim Ahmed S. A.

    2017-05-01

    Full Text Available Research designed to improve extraction has led to the development of microextraction techniques (ME, which involve simple, low cost, and effective preconcentrationof analytes in various matrices. This review is concerned with the principles and theoretical background of ME, as well as the development of applications for selenium analysis during the period from 2008 to 2016. Among all ME, dispersive liquid-liquid microextraction was found to be most favorable for selenium. On the other hand, atomic absorption spectrometry was the most frequently used instrumentation. Selenium ME have rarely been coupled to spectrophotometry and X-ray spectrophotometry methods, and there is no published application of ME with electrochemical techniques. We strongly support the idea of using a double preconcentration process, which consists of microextraction prior to preconcentration, followed by selenium determination using cathodic stripping voltammetry (ME-CSV. More attention should focus on the development of accurate, precise, and green methods for selenium analysis.

  20. Determination of Trichloroethylene in Water by Liquid–Liquid Microextraction Assisted Solid Phase Microextraction

    Directory of Open Access Journals (Sweden)

    Mengliang Zhang

    2015-02-01

    Full Text Available A method for the determination of trichloroethylene (TCE in water using portable gas chromatography/mass spectrometry (GC/MS was developed. A novel sample preparation method, liquid–liquid microextraction assisted solid phase microextraction (LLME–SPME, is introduced. In this method, 20 µL of hexane was added to 10 mL of TCE contaminated aqueous samples to assist headspace SPME. The extraction efficiency of SPME was significantly improved with the addition of minute amounts of organic solvents (i.e., 20 µL hexane. The absolute recoveries of TCE at different concentrations were increased from 11%–17% for the samples extracted by SPME to 29%–41% for the samples extracted by LLME–SPME. The method was demonstrated to be linear from 10 to 1000 ng mL−1 for TCE in water. The improvements on extraction efficiencies were also observed for toluene and 1, 2, 4-trichlorobenzene in water by using LLME–SPME method. The LLME–SPME method was optimized by using response surface modeling (RSM.

  1. Highly porous nanostructured copper foam fiber impregnated with an organic solvent for headspace liquid-phase microextraction.

    Science.gov (United States)

    Saraji, Mohammad; Ghani, Milad; Rezaei, Behzad; Mokhtarianpour, Maryam

    2016-10-21

    A new headspace liquid-phase microextraction technique based on using a copper foam nanostructure substrate followed by gas chromatography-flame ionization detection was developed for the determination of volatile organic compounds in water and wastewater samples. The copper foam with highly porous nanostructured walls was fabricated on the surface of a copper wire by a rapid and facile electrochemical process and used as the extractant solvent holder. Propyl benzoate was immobilized in the pores of the copper foam coating and used for the microextraction of benzene, toluene, ethylbenzene and xylenes. The experimental parameters such as the type of organic solvent, desorption temperature, desorption time, salt concentration, sample temperature, equilibrium time and extraction time, were investigated and optimized. Under the optimum conditions, the method detection limit was between 0.06 and 0.25μgL -1 . The relative standard deviation of the method for the analytes at 4-8μgL -1 concentration level ranged from 7.9 to 11%. The fiber-to-fiber reproducibility for three fibers prepared under the same condition was 9.3-12%. The enrichment factor was in the range of 615-744. Different water samples were analyzed for the evaluation of the method in real sample analysis. Relative recoveries for spiked tap, river and wastewater samples were in the range of 85-94%. Finally, the extraction efficiency of the method was compared with those of headspace single drop microextraction and headspace SPME with the commercial fibers. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. Sessile Drop Evaporation and Leidenfrost Phenomenon

    OpenAIRE

    A. K. Mozumder; M. R. Ullah; A. Hossain; M. A. Islam

    2010-01-01

    Problem statement: Quenching and cooling are important process in manufacturing industry for controlling the mechanical properties of materials, where evaporation is a vital mode of heat transfer. Approach: This study experimentally investigated the evaporation of sessile drop for four different heated surfaces of Aluminum, Brass, Copper and Mild steel with a combination of four different liquids as Methanol, Ethanol, Water and NaCl solution. The time of evaporation for the droplet on the hot...

  3. Gas Pressure-Drop Experiment

    Science.gov (United States)

    Luyben, William L.; Tuzla, Kemal

    2010-01-01

    Most chemical engineering undergraduate laboratories have fluid mechanics experiments in which pressure drops through pipes are measured over a range of Reynolds numbers. The standard fluid is liquid water, which is essentially incompressible. Since density is constant, pressure drop does not depend on the pressure in the pipe. In addition, flow…

  4. Hanging drop crystal growth apparatus

    Science.gov (United States)

    Naumann, Robert J. (Inventor); Witherow, William K. (Inventor); Carter, Daniel C. (Inventor); Bugg, Charles E. (Inventor); Suddath, Fred L. (Inventor)

    1990-01-01

    This invention relates generally to control systems for controlling crystal growth, and more particularly to such a system which uses a beam of light refracted by the fluid in which crystals are growing to detect concentration of solutes in the liquid. In a hanging drop apparatus, a laser beam is directed onto drop which refracts the laser light into primary and secondary bows, respectively, which in turn fall upon linear diode detector arrays. As concentration of solutes in drop increases due to solvent removal, these bows move farther apart on the arrays, with the relative separation being detected by arrays and used by a computer to adjust solvent vapor transport from the drop. A forward scattering detector is used to detect crystal nucleation in drop, and a humidity detector is used, in one embodiment, to detect relative humidity in the enclosure wherein drop is suspended. The novelty of this invention lies in utilizing angular variance of light refracted from drop to infer, by a computer algorithm, concentration of solutes therein. Additional novelty is believed to lie in using a forward scattering detector to detect nucleating crystallites in drop.

  5. Determination of arsenic and selenium by hydride generation and headspace solid phase microextraction coupled with optical emission spectrometry

    Science.gov (United States)

    Tyburska, Anna; Jankowski, Krzysztof; Rodzik, Agnieszka

    2011-07-01

    A hydride generation headspace solid phase microextraction technique has been developed in combination with optical emission spectrometry for determination of total arsenic and selenium. Hydrides were generated in a 10 mL volume septum-sealed vial and subsequently collected onto a polydimethylsiloxane/Carboxen solid phase microextraction fiber from the headspace of sample solution. After completion of the sorption, the fiber was transferred into a thermal desorption unit and the analytes were vaporized and directly introduced into argon inductively coupled plasma or helium microwave induced plasma radiation source. Experimental conditions of hydride formation reaction as well as sorption and desorption of analytes have been optimized showing the significant effect of the type of the solid phase microextraction fiber coating, the sorption time and hydrochloric acid concentration of the sample solution on analytical characteristics of the method developed. The limits of detection of arsenic and selenium were 0.1 and 0.8 ng mL - 1 , respectively. The limit of detection of selenium could be improved further using biosorption with baker's yeast Saccharomyces cerevisiae for analyte preconcentration. The technique was applied for the determination of total As and Se in real samples.

  6. Magnetic control of Leidenfrost drops.

    Science.gov (United States)

    Piroird, Keyvan; Clanet, Christophe; Quéré, David

    2012-05-01

    We show how a magnetic field can influence the motion of a paramagnetic drop made of liquid oxygen in a Leidenfrost state on solids at room temperature. It is demonstrated that the trajectory can be modified in both direction and velocity and that the results can be interpreted in terms of classical mechanics as long as the drop does not get too close to the magnet. We study the deviation and report that it can easily overcome 180∘ and even diverge under certain conditions, leading to situations where a drop gets captured. In the vicinity of the magnet, another type of trapping is observed, due to the deformation of the drop in this region, which leads to a strong energy dissipation. Conversely, drops can be accelerated by moving magnets (slingshot effect).

  7. Determination of Atrazine, Acetochlor, Clomazone, Pendimethalin and Oxyfluorfen in Soil by a Solid Phase Microextraction Method

    Directory of Open Access Journals (Sweden)

    Rada Đurović

    2008-01-01

    Full Text Available A solid phase microextraction (SPME method for simultaneous determination of atrazine, acetochlor, clomazone, pendimethalin and oxyfluorfen in soil samples was developed. The method is based on a combination of conventional liquid-solid procedure and a following SPME determination of the selected pesticides. Initially, various microextraction conditions, such as the fibre type, desorption temperature and time, extraction time and NaCl content, were investigated and optimized. Then, extraction efficiencies of severalsolvents (water, hexane, acetonitrile, acetone and methanol and the optimum number of extraction steps within the sample preparation step were optimized. According to the results obtained in these two sets of experiments, two successive extractions with methanol as the extraction solvent were the optimal sample preparation procedure, while the following conditions were found to be most efficient for SPME measurements: 100 μm PDMS fibre, desorption for 7 min at 2700C, 30 min extraction time and 5% NaCl content (w/v. Detection and quantification were done by gas chromatography-mass spectrometry(GC/MS. Relative standard deviation (RSD values for multiple analysis of soil samples fortified at 30 μg/kg of each pesticide were below 19%. Limits of detection (LOD for all the compounds studied were less than 2 μg/kg.

  8. Pool impacts of Leidenfrost drop

    Science.gov (United States)

    Darbois Texier, Baptiste; Maquet, Laurent; Dorbolo, Stephane; Dehandschoewercker, Eline; Pan, Zhao; Truscott, Tadd

    2015-11-01

    This work concerns the impact of a droplet made of a volatile liquid (typically HFE) on a pool of an other liquid (typically silicone oil) which temperature is above the boiling point of the drop. Depending on the properties of the two liquids and the impacting conditions, four different regimes are observed. For low impacting speeds, the droplet bounces on the surface of the bath and finally levitates above it in a Leidenfrost state. Such a regime occurs as soon as the pool temperature exceeds the boiling point of the drop. This observation means that there is no threshold in temperature for a Leidenfrost effect on a liquid surface contrary to the case of a solid substrate. For intermediate impacting velocities, the pinch-off of the surface of the pool entraps the drop in the liquid bulk. The entrapped drop is separated from the pool by a layer of its own vapour in a similar way of antibulles. For increasing impacting speeds, the vapour layer between the drop and the pool does not hold during the pinch-off event. The contact of the drop with the hot liquid provokes a sudden and intense evaporation. At very large impacting speeds, the drop rapidely contacts the pool, spreads and finally induces a hemi-spherical cavity. In the end, these four different regimes are summarized in a Froud-Weber diagram which boundaries are discussed.

  9. Trapping leidenfrost drops with crenelations.

    Science.gov (United States)

    Dupeux, Guillaume; Le Merrer, Marie; Clanet, Christophe; Quéré, David

    2011-09-09

    Drops placed on very hot solids levitate on a cushion of their own vapor, as discovered by Leidenfrost. This confers to these drops a remarkable mobility, which makes problematic their control and manipulation. Here we show how crenelated surfaces can be used to increase the friction of Leidenfrost drops by a factor on the order of 100, making them decelerate and be trapped on centimetric distances instead of the usual metric ones. We measure and characterize the friction force as a function of the design of the crenelations.

  10. Tunable transport of drops on a vibrating inclined fiber

    Science.gov (United States)

    Bick, Alison; Boulogne, François; Sauret, Alban; Stone, Howard A.

    2015-11-01

    Transport of liquid drops in fibrous media occurs in various engineering systems such as fog harvesting or cleaning of textiles. The ability to tune or to control liquid movement can increase the system efficiency and enable new engineering applications. In this letter, we experimentally investigate how partially wetting drops on a single fiber can be manipulated by vibrating the fiber. We show that a sliding motion along the fiber or a dripping of the drop can be triggered by standing waves. We identify the conditions on the drop volume, the fiber tilt angle, and the amplitude and frequency of oscillations to observe these different behaviors. Finally, we experimentally illustrate that vibrations can be used to control the transport and the collection of water drops along a fiber using a combination of the sliding and dripping transitions.

  11. Headspace solid-phase microextraction and gas chromatography ...

    African Journals Online (AJOL)

    Purpose: To extract and analyze the volatile components of Chrysanthemum morifolium Ramat. 'huaiju' by headspace solid-phase microextraction (HS-SPME) and gas chromatography–mass spectrometry. (GC–MS). Methods: Volatile components were extracted by HS-SPME and identified by GC–MS. The relative contents ...

  12. Solid-phase microextraction for the analysis of biological samples

    NARCIS (Netherlands)

    Theodoridis, G; Koster, EHM; de Jong, GJ

    2000-01-01

    Solid-phase microextraction (SPME) has been introduced for the extraction of organic compounds from environmental samples. This relatively new extraction technique has now also gained a lot of interest in a broad field of analysis including food, biological and pharmaceutical samples. SPME has a

  13. Headspace solid-phase microextraction and gas chromatography ...

    African Journals Online (AJOL)

    Purpose: To extract and analyze the volatile components of Chrysanthemum morifolium Ramat. 'huaiju' by headspace solid-phase microextraction (HS-SPME) and gas chromatography–mass spectrometry (GC–MS). Methods: Volatile components were extracted by HS-SPME and identified by GC–MS. The relative contents ...

  14. Development of headspace solid-phase microextraction method for ...

    African Journals Online (AJOL)

    ... analysis of 14 multiclass pesticide residues in fruits and vegetable samples. The gas chromatography mass spectrometry parameters (desorption temperature and time, column flow rate, interface temperature) and solid phase microextraction parameters (fiber coating type, extraction temperature and time, pH, salt addition ...

  15. 45-FOOT HIGH DROP TOWER

    Data.gov (United States)

    Federal Laboratory Consortium — The Drop Tower is used to simulate and measure the impact shocks that are exerted on parachute loads when they hit the ground. It is also used for HSL static lift to...

  16. Application of solid-phase microextraction in analytical toxicology.

    Science.gov (United States)

    Pragst, Fritz

    2007-08-01

    Solid-phase microextraction (SPME) is a miniaturized and solvent-free sample preparation technique for chromatographic-spectrometric analysis by which the analytes are extracted from a gaseous or liquid sample by absorption in, or adsorption on, a thin polymer coating fixed to the solid surface of a fiber, inside an injection needle or inside a capillary. In this paper, the present state of practical performance and of applications of SPME to the analysis of blood, urine, oral fluid and hair in clinical and forensic toxicology is reviewed. The commercial coatings for fibers or needles have not essentially changed for many years, but there are interesting laboratory developments, such as conductive polypyrrole coatings for electrochemically controlled SPME of anions or cations and coatings with restricted-access properties for direct extraction from whole blood or immunoaffinity SPME. In-tube SPME uses segments of commercial gas chromatography (GC) capillaries for highly efficient extraction by repeated aspiration-ejection cycles of the liquid sample. It can be easily automated in combination with liquid chromatography but, as it is very sensitive to capillary plugging, it requires completely homogeneous liquid samples. In contrast, fiber-based SPME has not yet been performed automatically in combination with high-performance liquid chromatography. The headspace extractions on fibers or needles (solid-phase dynamic extraction) combined with GC methods are the most advantageous versions of SPME because of very pure extracts and the availability of automatic samplers. Surprisingly, substances with quite high boiling points, such as tricyclic antidepressants or phenothiazines, can be measured by headspace SPME from aqueous samples. The applicability and sensitivity of SPME was essentially extended by in-sample or on-fiber derivatization. The different modes of SPME were applied to analysis of solvents and inhalation narcotics, amphetamines, cocaine and metabolites

  17. Shaping drops with textured surfaces

    Science.gov (United States)

    Ehlinger, Quentin; Biance, Anne-Laure; Ybert, Christophe

    2017-11-01

    When a drop impacts a substrate, it can behave differently depending on the nature of the surface and of the liquid (spreading, bouncing, resting, splashing ...). Understanding these behaviors is crucial to predict the drop morphology during and after impact. Whereas surface wettability has extensively been studied, the effect of surface roughness remains hardly explored. In this work, we consider the impact of a drop in a pure non-wetting situation by using superheated substrates i.e. in the Leidenfrost regime. The surface texture consists of a well-controlled microscopic defect shaped with photolithography on a smooth silicon wafer. Different regimes are observed, depending on the distance between the defect and the impact point and the defect size. Comparing the lamella thickness versus the defect height proves relevant as the transition criteria between regimes. Others characteristics of the drop behavior (direction of satellite droplet ejection, lamella rupture) are also well captured by inertial/capillary models. Drop impacts on multiple defects are also investigated and drop shape well predicted considering the interactions between the local flow and the defects.

  18. Comparison of solid phase microextraction and hollow fiber liquid phase microextraction for the determination of pesticides in aqueous samples by gas chromatography triple quadrupole tandem mass spectrometry.

    Science.gov (United States)

    Garrido Frenich, Antonia; Romero-González, R; Martínez Vidal, José Luis; Martínez Ocaña, R; Baquero Feria, P

    2011-02-01

    This work compares two miniaturised sample preparation methods, solid phase microextraction (SPME) and hollow fiber liquid phase microextraction (HF-LPME), in combination with gas chromatography coupled to tandem mass spectrometry with a triple quadrupole analyzer for the determination of 77 pesticides in drinking water. In the case of SPME, extraction temperature and time were optimized by experimental design, although other parameters, as desorption time, pH, and ionic strength, were also evaluated. The extraction and desorption solvents [octanol/dihexyl ether (75:25, v/v) and cyclohexane, respectively], as well as the extraction and desorption time, ionic strength, and pH, were studied for the HF-LPME procedure. Under the optimal conditions, recoveries (70.2-113.5% for SPME and 70.0-119.5% for HF-LPME), intra-day precision (2.1-19.4% for SPME and 4.3-22.5% for HF-LPME), inter-day precision (5.2-21.5% for SPME and 8.4-27.3% for HF-LPME), and limits of detection, between 0.1 and 28.8 ng/L for SPME and 0.2 and 47.1 ng/L for HF-LPME and overall uncertainty (9.6-25.2% for SPME and 13.3-27.5% for HF-LPME) were established for both extraction procedures. Finally, the proposed methods were successfully applied to the analysis of 41 drinking water samples, and similar results were obtained with both extraction approaches.

  19. Air sampling with solid phase microextraction

    Science.gov (United States)

    Martos, Perry Anthony

    There is an increasing need for simple yet accurate air sampling methods. The acceptance of new air sampling methods requires compatibility with conventional chromatographic equipment, and the new methods have to be environmentally friendly, simple to use, yet with equal, or better, detection limits, accuracy and precision than standard methods. Solid phase microextraction (SPME) satisfies the conditions for new air sampling methods. Analyte detection limits, accuracy and precision of analysis with SPME are typically better than with any conventional air sampling methods. Yet, air sampling with SPME requires no pumps, solvents, is re-usable, extremely simple to use, is completely compatible with current chromatographic equipment, and requires a small capital investment. The first SPME fiber coating used in this study was poly(dimethylsiloxane) (PDMS), a hydrophobic liquid film, to sample a large range of airborne hydrocarbons such as benzene and octane. Quantification without an external calibration procedure is possible with this coating. Well understood are the physical and chemical properties of this coating, which are quite similar to those of the siloxane stationary phase used in capillary columns. The log of analyte distribution coefficients for PDMS are linearly related to chromatographic retention indices and to the inverse of temperature. Therefore, the actual chromatogram from the analysis of the PDMS air sampler will yield the calibration parameters which are used to quantify unknown airborne analyte concentrations (ppb v to ppm v range). The second fiber coating used in this study was PDMS/divinyl benzene (PDMS/DVB) onto which o-(2,3,4,5,6- pentafluorobenzyl) hydroxylamine (PFBHA) was adsorbed for the on-fiber derivatization of gaseous formaldehyde (ppb v range), with and without external calibration. The oxime formed from the reaction can be detected with conventional gas chromatographic detectors. Typical grab sampling times were as small as 5 seconds

  20. Faster multiple emulsification with drop splitting.

    Science.gov (United States)

    Abate, Adam R; Weitz, David A

    2011-06-07

    Microfluidic devices can form emulsions in which the drops have an intricate, controlled structure; however, a challenge is that the droplets are produced slowly, typically only a few millilitres per hour. Here, we present a simple technique to increase the production rate. Using a large drop maker, we produce large drops at a fast volumetric rate; by splitting these drops several times in a splitting array, we create drops of the desired small size. The advantage of this over forming the small drops directly using a small drop maker is that the drops can be formed at much faster rates. This can be applied to the production of single and multiple emulsions.

  1. Thermocapillary reorientation of Janus drops

    Science.gov (United States)

    Rosales, Rodolfo; Saenz, Pedro

    2017-11-01

    Janus drops, named after the Ancient Roman two-faced god, are liquid drops formed from two immiscible fluids. Experimental observations indicate that a Janus drop may re-orientate in response to an applied external thermal gradient due to the Marangoni effect. Depending on the angle between the interior interface and the direction of the temperature gradient, disparities in the physical properties of the constituent liquids may lead to asymmetries in the thermocapillary flow. As a result, the drop will move along a curved path until a torque-free configuration is achieved, point after which it will continue on a straight trajectory. Here, we present the results of a theoretical investigation of this realignment phenomenon in the Stokes regime and in the limit of non-deformable interfaces. A 3D semi-analytical method in terms of polar spherical harmonics is developed to characterize and rationalize the hydrodynamic response (forces and torques), flow (velocity and temperature distribution) and trajectory of a Janus drop moving during the temperature-driven reorientation process. Furthermore, we discuss how this phenomenon may be exploited to develop dynamically reconfigurable micro-lenses. This work was partially supported by the US National Science Foundation through Grants DMS-1614043 and DMS-1719637.

  2. Drop entrainment from the surface of oil mist filters: mechanisms, kinetics, and drop spectra

    OpenAIRE

    Wurster, S.; Kolb, H.; Meyer, J.; Kasper, G.

    2016-01-01

    Oil entrainment from coalescence filters has been characterized by different techniques. Drop spectra and entrainment rates were measured by a combination of techniques from 1 mm over long periods of time. Dominant entrainment mechanism(s) are identified on the basis of comparisons of entrainment rates measured in different regions of the filter surface with rates of air bubble formation, measurements of oil film thickness, as well as visual observations. Experiments are supported by force es...

  3. Interfacial Instabilities in Evaporating Drops

    Science.gov (United States)

    Moffat, Ross; Sefiane, Khellil; Matar, Omar

    2007-11-01

    We study the effect of substrate thermal properties on the evaporation of sessile drops of various liquids. An infra-red imaging technique was used to record the interfacial temperature. This technique illustrates the non-uniformity in interfacial temperature distribution that characterises the evaporation process. Our results also demonstrate that the evaporation of methanol droplets is accompanied by the formation of wave-trains in the interfacial temperature field; similar patterns, however, were not observed in the case of water droplets. More complex patterns are observed for FC-72 refrigerant drops. The effect of substrate thermal conductivity on the structure of the complex pattern formation is also elucidated.

  4. Determination of parabens using two microextraction methods coupled with capillary liquid chromatography-UV detection.

    Science.gov (United States)

    Chen, Chen-Wen; Hsu, Wen-Chan; Lu, Ya-Chen; Weng, Jing-Ru; Feng, Chia-Hsien

    2018-02-15

    Parabens are common preservatives and environmental hormones. As such, possible detrimental health effects could be amplified through their widespread use in foods, cosmetics, and pharmaceutical products. Thus, the determination of parabens in such products is of particular importance. This study explored vortex-assisted dispersive liquid-liquid microextraction techniques based on the solidification of a floating organic drop (VA-DLLME-SFO) and salt-assisted cloud point extraction (SA-CPE) for paraben extraction. Microanalysis was performed using a capillary liquid chromatography-ultraviolet detection system. These techniques were modified successfully to determine four parabens in 19 commercial products. The regression equations of these parabens exhibited good linearity (r 2 =0.998, 0.1-10μg/mL), good precision (RSD<5%) and accuracy (RE<5%), reduced reagent consumption and reaction times (<6min), and excellent sample versatility. VA-DLLME-SFO was also particularly convenient due to the use of a solidified extract. Thus, the VA-DLLME-SFO technique was better suited to the extraction of parabens from complex matrices. Copyright © 2017 Elsevier Ltd. All rights reserved.

  5. Heat exchange between a bouncing drop and a superhydrophobic substrate.

    Science.gov (United States)

    Shiri, Samira; Bird, James C

    2017-07-03

    The ability to enhance or limit heat transfer between a surface and impacting drops is important in applications ranging from industrial spray cooling to the thermal regulation of animals in cold rain. When these surfaces are micro/nanotextured and hydrophobic, or superhydrophobic, an impacting drop can spread and recoil over trapped air pockets so quickly that it can completely bounce off the surface. It is expected that this short contact time limits heat transfer; however, the amount of heat exchanged and precise role of various parameters, such as the drop size, are unknown. Here, we demonstrate that the amount of heat exchanged between a millimeter-sized water drop and a superhydrophobic surface will be orders of magnitude less when the drop bounces than when it sticks. Through a combination of experiments and theory, we show that the heat transfer process on superhydrophobic surfaces is independent of the trapped gas. Instead, we find that, for a given spreading factor, the small fraction of heat transferred is controlled by two dimensionless groupings of physical parameters: one that relates the thermal properties of the drop and bulk substrate and the other that characterizes the relative thermal, inertial, and capillary dynamics of the drop.

  6. STUDY ON SOFTENING AND DROPPING PROPERTIES OF METALIZED BURDEN INSIDE BLAST FURNACE

    Directory of Open Access Journals (Sweden)

    Bi-yang Tuo

    2014-12-01

    Full Text Available The inferences of burden metallization rate on softening-melting dropping properties were investigated through softening-melting dropping test of three kinds of metalized burden pressure drop. The results indicated that the softeningmelting temperature interval of pre-reduction mixed burden is bigger than primeval mixed burden, the melting interval narrow with the rise of metallization rate of ferric burden as well as dropping temperature interval. The average pressure drop, maximum pressure drop and softening-melting dropping properties eigenvalue decrease with the rise of metallization rate of ferric burden. Besides, the dropping temperature of burden reduces with the rise of carbon content of molten iron. The combination high metalized burden and higher carbon content of molten iron is benefit to decreasing thickness of cohesive zone and improve permeability of cohesive zone.

  7. Automation and optimization of liquid-phase microextraction by gas chromatography.

    Science.gov (United States)

    Ouyang, Gangfeng; Zhao, Wennan; Pawliszyn, Janusz

    2007-01-05

    Several fully automated liquid-phase microextraction (LPME) techniques, including static headspace LPME (HS-LPME) (a drop of solvent is suspended at the tip of a microsyringe needle and exposed to the headspace of the sample solution), exposed dynamic HS-LPME (the solvent is exposed in the headspace of sample vial for different time, and then withdrawn into the barrel of the syringe. This procedure is repeated a number of times), unexposed dynamic HS-LPME (the solvent is moved inside the needle and the barrel of a syringe, and the gaseous sample is withdrawn into the barrel and then ejected), static direct-immersed LPME (DI-LPME) (a drop of solvent is suspended at the tip of a microsyringe needle and directly immersed into the sample solution), dynamic DI-LPME (the solvent is moved inside the needle and the barrel of a syringe, and the sample solution is withdrawn and ejected), and two phase hollow fiber-protected LPME (HF-LPME) (a hollow fiber is used to stabilize and protect the solvent), auto-performed with a commercial CTC CombiPal autosampler, are described in this paper. Critical experimental factors, including temperature, choice of extraction solvent, solvent volume, plunger movement rate, and extraction time were investigated. Among the three HS-LPME techniques that were evaluated, the exposed dynamic HS-LPME technique provided the best performance, compared to the unexposed dynamic HS-LPME and static HS-LPME approaches. For DI-LPME, the dynamic process can enhance the extraction efficiency and the achieved method precision is comparable with the static DI-LPME technique. The precision of the fully automated HF-LPME is quite acceptable (RSD values below 6.8%), and the concentration enrichment factors are better than the DI-LPME approaches. The fully automated LPME techniques are more accurate and more convenient, and the reproducibility achieved eliminates the need for an internal standard to improve the method precision.

  8. Pressure drop in contraction flow

    DEFF Research Database (Denmark)

    Rasmussen, Henrik Koblitz

    This note is a supplement to Dynamic of Polymeric Liquids (DPL) page 178. DPL gives an equation for the pressure drop in a tapered (and circular) contraction, valid only at low angles. Here the general definition of contraction flow (the Bagley correction) and a more general method to find...

  9. Fluid flow in drying drops

    NARCIS (Netherlands)

    Gelderblom, Hanneke

    2013-01-01

    When a suspension drop evaporates, it leaves behind a drying stain. Examples of these drying stains encountered in daily life are coffee or tea stains on a table top, mineral rings on glassware that comes out of the dishwasher, or the salt deposits on the streets in winter. Drying stains are also

  10. Drops, contact lines, and electrowetting

    NARCIS (Netherlands)

    't Mannetje, Dieter

    2013-01-01

    In this work, we study the behaviour of drops and contact lines under the influence of electric fields, and how these can answer fundamental and industrial questions. Our focus is on studying the varying balance of the electric field, hysteresis forces and inertia as the speed of a contact line

  11. Monitoring Pb in Aqueous Samples by Using Low Density Solvent on Air-Assisted Dispersive Liquid-Liquid Microextraction Coupled with UV-Vis Spectrophotometry.

    Science.gov (United States)

    Nejad, Mina Ghasemi; Faraji, Hakim; Moghimi, Ali

    2017-04-01

    In this study, AA-DLLME combined with UV-Vis spectrophotometry was developed for pre-concentration, microextraction and determination of lead in aqueous samples. Optimization of the independent variables was carried out according to chemometric methods in three steps. According to the screening and optimization study, 86 μL of 1-undecanol (extracting solvent), 12 times syringe pumps, pH 2.0, 0.00% of salt and 0.1% DDTP (chelating agent) were chosen as the optimum independent variables for microextraction and determination of lead. Under the optimized conditions, R = 0.9994, and linearity range was 0.01-100 µg mL -1 . LOD and LOQ were 3.4 and 11.6 ng mL -1 , respectively. The method was applied for analysis of real water samples, such as tap, mineral, river and waste water.

  12. Development of a coupled dispersive liquid-liquid micro-extraction ...

    African Journals Online (AJOL)

    However, the results demonstrated the potential of this method in determination of triclosan in water-based samples when the extraction was coupled to a more rugged system such as a GC-MS. Keywords: dispersive liquid-liquid microextraction, liquid phase microextraction, coupling, mixed-solvents, triclosan, wastewater.

  13. Recent progress, challenges and trends in trace determination of drug analysis using molecularly imprinted solid-phase microextraction technology.

    Science.gov (United States)

    Ansari, Saeedeh; Karimi, Majid

    2017-03-01

    The quantification of drugs in biological samples is a significant task for determination of the physiological efficiency in evaluated drugs in the drug discovery. To analysis of the chemical compounds at the trace and ultratrace levels, adequate analytical procedures should be applied. Therefore, sample preparation method undoubtedly is the most important stage in the trace determination process. In spite of the great growth of analytical instrumentation during the recent years, sample preparation is still nowadays considered the impasse of the all analytical procedure, especially in drugs analysis. Because of the low concentration level of drugs in blood, plasma, and the diversity of the metabolites, the chosen extraction technique should be almost perfect. Solid-phase microextraction (SPME) is a powerful, simple, fast and an equilibrium-based sample preparation method that permits integration of sampling, sample clean-up, and pre-concentration in a single solvent-free step for chemical analysis. Molecularly imprinted polymers (MIPs) that provided by the presence of a template during their synthesis are the stable polymers with molecular recognition abilities and excellent materials which provide selectivity to sample preparation. Because of its characteristics such as easy preparation, high selectivity, and chemical stability, MIP is widely utilized in many analytical fields. Accordingly, the molecular imprinting and SPME methods combination would prepare a strong analytical instrumentation which comprises simplicity, flexibility, and the selectivity characteristics of both methods. This review focuses on the application of solid-phase microextraction method coupled with molecularly imprinted polymers, namely molecularly imprinted solid-phase microextraction (MISPME), for trace determination in drug analysis. Copyright © 2016 Elsevier B.V. All rights reserved.

  14. Evaluation of in vivo solid phase microextraction for minimally invasive analysis of nonvolatile phytochemicals in Amazonian plants.

    Science.gov (United States)

    Musteata, Florin Marcel; Sandoval, Manuel; Ruiz-Macedo, Juan C; Harrison, Kathleen; McKenna, Dennis; Millington, William

    2016-08-24

    Although solid phase microextraction (SPME) has been used extensively for fingerprinting volatile compounds emitted by plants, there are very few such reports for direct insertion SPME. In this research, direct contact of SPME probes with the interstitial fluid of plants was investigated as a method for phytochemical analysis. Medicinal plants from the Amazon have been the source of numerous drugs used in western medicine. However, a large number of species used in traditional medicine have not been characterized chemically, partly due to the difficulty of field work. In this project, the phytochemical composition of plants from several genera was fingerprinted by combining convenient field sampling by solid phase microextraction (SPME) with laboratory analysis by LC-MS. The new method was compared with classical sampling followed by liquid extraction (LE). SPME probes were prepared by coating stainless steel wires with a mixture of polyacrylonitrile and either RP-amide or HS-F5 silica particles. Sampling was performed by inserting the microextraction probes into various tissues of living plants in their natural environment. After in vivo extraction, the probes were sealed under vacuum and refrigerated until analyzed. The probes were desorbed in mobile phase and analyzed on a Waters Acquity UPLC with triple quadrupole mass spectrometer in positive ion mode. Twenty Amazonian plant species were sampled and unique metabolomic fingerprints were obtained. In addition, quantitative analysis was performed for previously identified compounds in three species. Comparison of the fingerprints obtained by in vivo SPME with those obtained by LE showed that 27% of the chromatographic features were unique to SPME, 57% were unique to LE, and 16% were common to both methods. In vivo SPME caused minimal damage to the plants, was much faster than traditional liquid extraction, and provided unique fingerprints for all investigated plants. SPME revealed unique chromatographic

  15. Device for making liquid drops

    International Nuclear Information System (INIS)

    Yamada, Masao; Fukuda, Fumito; Nishikawa, Masana; Ishii, Takeshi.

    1976-01-01

    Object: To provide a device for producing liquid drops in the form of liquefied gases indispensable to make deuterium and tritium ice pellets used as a fusion fuel in a tokamak type fusion reactor. Structure: First, pressure P 1 at the upper surface of liquefied gas in a container and outlet pressure P 2 of a nozzle disposed at the lower part of the container are adjusted into the state of P 1 >= P 2 , and it is preset so that even under such conditions, the liquefied gas from the nozzle is not naturally flown out. Next, a vibration plate disposed within the container is rapidly downwardly advanced toward the nozzle through a predetermined distance. As a result, pressure of the liquefied gas within a depression under the vibration plate rises instantaneously or in a pulse fashion to dissatisfy the aforesaid set condition whereby the liquefied gas may be flown out from the nozzle in the form of liquid drops. In accordance with the present device, it is possible to produce a suitable number of drops at a suitable point. (Yoshihara, H.)

  16. Dancing drops over vibrating substrates

    Science.gov (United States)

    Borcia, Rodica; Borcia, Ion Dan; Helbig, Markus; Meier, Martin; Egbers, Christoph; Bestehorn, Michael

    2017-04-01

    We study the motion of a liquid drop on a solid plate simultaneously submitted to horizontal and vertical harmonic vibrations. The investigation is done via a phase field model earlier developed for describing static and dynamic contact angles. The density field is nearly constant in every bulk region (ρ = 1 in the liquid phase, ρ ≈ 0 in the vapor phase) and varies continuously from one phase to the other with a rapid but smooth variation across the interfaces. Complicated explicit boundary conditions along the interface are avoided and captured implicitly by gradient terms of ρ in the hydrodynamic basic equations. The contact angle θ is controlled through the density at the solid substrate ρ S , a free parameter varying between 0 and 1 [R. Borcia, I.D. Borcia, M. Bestehorn, Phys. Rev. E 78, 066307 (2008)]. We emphasize the swaying and the spreading modes, earlier theoretically identified by Benilov and Billingham via a shallow-water model for drops climbing uphill along an inclined plane oscillating vertically [E.S. Benilov, J. Billingham, J. Fluid Mech. 674, 93 (2011)]. The numerical phase field simulations will be completed by experiments. Some ways to prevent the release of the dancing drops along a hydrophobic surface into the gas atmosphere are also discussed in this paper.

  17. Anomalous water drop bouncing on a nanotextured surface by the Leidenfrost levitation

    Science.gov (United States)

    Lee, Doo Jin; Song, Young Seok

    2016-05-01

    We report an anomalous liquid drop bouncing phenomenon that is generated by the Leidenfrost levitation due to a vapor layer reducing energy dissipation during the collision. The Leidenfrost levitation of water drops on both a hydrophobic surface and nanotextured Cassie surface is investigated. When the water drop is positioned onto the hydrophobic surface, a superhydrophobic feature is observed by the levitation effect due to the vapor film, which results in a slow evaporation of the drop due to the low thermal conductivity of the vapor layer that inhibits heat transfer between the heated surface and the water drop. In contrast, for the nanotextured surface, the water drop can bounce off after impact on the surface when it overcomes gravitational and adhesion forces. The spontaneous water drop bouncing on the nanotextured surface is powered by the combination effect of the Leidenfrost levitation and the non-wetting Cassie state.

  18. Ionic liquid-linked dual magnetic microextraction of lead(II) from environmental samples prior to its micro-sampling flame atomic absorption spectrometric determination.

    Science.gov (United States)

    Yilmaz, Erkan; Soylak, Mustafa

    2013-11-15

    A novel and rapid microextraction approach termed as ionic liquid-linked dual magnetic microextraction (IL-DMME), was developed for the atomic absorption spectrometric determination of lead. The developed method based on a combination of dispersive liquid-liquid microextraction (DLLME) and dispersive micro solid-phase extraction (D-μ-SPE). In the first DLLME step, 1-butyl-3-methylimidazolium hexafluorophosphate [C4mim][PF6], was selected to extract the lead-pyrrolidine-dithiocarbamate (Pb-PDC) complex from sample solution by the assistance of vortex agitator. After the first step, fifty milligrams of Fe3O4 magnetic nanoparticles (MNPs) were added to extraction of the ionic liquid and Pb-PDC complex in aqueous solution. The effective factors in proposed IL-DMME procedure, including volume of 1-butyl-3-methylimidazolium hexafluorophosphate, amount of Fe3O4 magnetic nanoparticles, vortex time, amount of ammonium pyrrolidinedithiocarbamate, sample volume and matrix effect were optimized in details. Under the optimal conditions, the method present has low detection limit (0.57 μg L(-1)), high preconcentration factor (160) and good repeatability (analysis of the certified reference materials and addition-recovery tests. The method was successfully applied to the determination of lead in water, plant and hair samples. © 2013 Elsevier B.V. All rights reserved.

  19. Experimental Research on Thermocapillary-Buoyancy Migration Interaction of Axisymmetric Two Drops by Using Digital Holographic Interferometry

    Science.gov (United States)

    Zhang, Shuoting; Duan, Li; Kang, Qi

    2017-12-01

    The migration and interaction of axisymmetric two drops in a vertical temperature gradient is investigated experimentally on the ground. A silicon oil is used as the continuous phase, and a water-ethanol mixture is used as the drop phase, respectively. The migration and interaction of two drops, under the combined effects of buoyancy and thermocapillary, is recorded by a digital holographic interferometry measurement in the experiment to analyse the velocities and temperature distribution of the drops. As a result, when two drops migrate together, the drop affects the other drop by perturbing the temperature field around itself. For the leading drop, the velocity is faster than the one of the isolated drop, and the maximum of the interfacial temperature distribution is larger than the one of the isolated drop. For the trailing drop, the velocity is slower than the one of the isolated drop, and the maximum of the interfacial temperature distribution is less than the one of the isolated drop. The influence of the dimensionless initial distance between the drop centres to the drop migration is discussed in detail in this study.

  20. Drag and drop display & builder

    Energy Technology Data Exchange (ETDEWEB)

    Bolshakov, Timofei B.; Petrov, Andrey D.; /Fermilab

    2007-12-01

    The Drag and Drop (DnD) Display & Builder is a component-oriented system that allows users to create visual representations of data received from data acquisition systems. It is an upgrade of a Synoptic Display mechanism used at Fermilab since 2002. Components can be graphically arranged and logically interconnected in the web-startable Project Builder. Projects can be either lightweight AJAX- and SVG-based web pages, or they can be started as Java applications. The new version was initiated as a response to discussions between the LHC Controls Group and Fermilab.

  1. Drop splashing is independent of substrate wetting

    Science.gov (United States)

    Latka, Andrzej; Boelens, Arnout M. P.; Nagel, Sidney R.; de Pablo, Juan J.

    2018-02-01

    A liquid drop impacting a dry solid surface with sufficient kinetic energy will splash, breaking apart into numerous secondary droplets. This phenomenon shows many similarities to forced wetting, including the entrainment of air at the contact line. Because of these similarities and the fact that forced wetting has been shown to depend on the wetting properties of the surface, existing theories predict splashing to depend on wetting properties as well. However, using high-speed interference imaging, we observe that at high capillary numbers wetting properties have no effect on splashing for various liquid-surface combinations. Additionally, by fully resolving the Navier-Stokes equations at length and time scales inaccessible to experiments, we find that the shape and motion of the air-liquid interface at the contact line/edge of the droplet are independent of wettability. We use these findings to evaluate existing theories and to compare splashing with forced wetting.

  2. Headspace thin-film microextraction onto graphene membranes for specific detection of methyl(cyclopentadienyl)-tricarbonyl manganese in water samples by total reflection X-ray fluorescence

    Science.gov (United States)

    Romero, V.; Costas-Mora, I.; Lavilla, I.; Bendicho, C.

    2016-12-01

    In this work, a novel analytical approach for determining methyl(cyclopentadienyl)-tricarbonyl (MMT) by total reflection X-ray fluorescence (TXRF) based on its trapping onto unmodified graphene membranes is described. Graphene membranes were synthesized by mild-thermal reduction of graphene oxide following drop-casting onto a glass substrate. High flexible and easy-to-handle graphene membranes with 10 mm diameter were obtained. In order to use the as-prepared membranes as extraction phases for headspace thin-solid film microextraction of MMT, they were fitted to quartz reflectors and placed onto the top of the glass vial containing the sample. Reflectors containing graphene membranes were directly used as sample carriers for TXRF analysis. Different parameters involved in the microextraction step were optimized in order to obtain the best performance. Detection and quantification limits were 18 and 60 ng L- 1 MMT, respectively. An enrichment factor of 265 was obtained. The method was successfully applied for the specific detection of MMT in different water samples and a certified reference material e.g., NWTM-27.2 fortified lake water. A recovery study was carried out on spiked water samples showing recoveries in the range 98-104% with a relative standard deviation of 4% (N = 5). In addition, speciation of manganese, i.e. MMT and Mn(II),in water samples can be accomplished since only volatile MMT is transferred to the headspace and retained onto graphene membranes.

  3. Determination of multi-class herbicides in soil by liquid-solid extraction coupled with headspace solid phase microextraction method

    Directory of Open Access Journals (Sweden)

    Đurović-Pejčev Rada

    2016-01-01

    Full Text Available A method is described for simultaneous determination of five herbicides (metribuzin, acetochlor, clomazone, oxyfluorfen and dimethenamid belonging to different pesticides groups in soil samples. Developed headspace solid phase microextraction method (HS-SPME in combination with liquid-solid sample preparation (LS was optimized and applied in the analysis of some agricultural samples. Optimization of microextraction conditions, such as temperature, extraction time and sodium chloride (NaCl content was perfor-med using 100 μm polydimethyl-siloxane (PDMS fiber. The extraction effi-ciencies of methanol, methanol:acetone=1:1 and methanol:acetone:hexane= =2:2:1 and the optimum number of extraction steps during the sample prepa-ration, were tested, as well. Gas chromatography-mass spectrometry (GC-MS was used for detection and quantification, obtaining relative standard deviation (RSD below 13%, and recovery values higher than 83% for multiple analyses of soil samples fortified at 30 μg kg-1 of each herbicide. Limits of detection (LOD were less than 1.2 μg kg-1 for all the studied herbicides. [Projekat Ministarstva nauke Republike Srbije, br. TR31043 i br. III43005

  4. Vibration-Induced Climbing of Drops

    Science.gov (United States)

    Brunet, P.; Eggers, J.; Deegan, R. D.

    2007-10-01

    We report an experimental study of liquid drops moving against gravity, when placed on a vertically vibrating inclined plate, which is partially wetted by the drop. The frequency of vibrations ranges from 30 to 200 Hz, and, above a threshold in vibration acceleration, drops experience an upward motion. We attribute this surprising motion to the deformations of the drop, as a consequence of an up or down symmetry breaking induced by the presence of the substrate. We relate the direction of motion to contact angle measurements. This phenomenon can be used to move a drop along an arbitrary path in a plane, without special surface treatments or localized forcing.

  5. Drop splashing: the role of surface wettability and liquid viscosity

    Science.gov (United States)

    Almohammadi, Hamed; Amirfazli, Alidad; -Team

    2017-11-01

    There are seemingly contradictory results in the literature about the role of surface wettability and drop viscosity for the splashing behavior of a drop impacting onto a surface. Motivated by such issues, we conducted a systematic experimental study where splashing behavior for a wide range of the liquid viscosity (1-100 cSt) and surface wettability (hydrophilic to hydrophobic) are examined. The experiments were performed for the liquids with both low and high surface tensions ( 20 and 72 mN/m). We found that the wettability affects the splashing threshold at high or low contact angle values. At the same drop velocity, an increase of the viscosity (up to 4 cSt) promotes the splashing; while, beyond such value, any increase in viscosity shows the opposite effect. It is also found that at a particular combination of liquid surface tension and viscosity (e.g. silicone oil, 10 cSt), an increase in the drop velocity changes the splashing to spreading. We relate such behaviors to the thickness, shape, and the velocity of the drop's lamella. Finally, to predict the splashing, we developed an empirical correlation which covers all of the previous reported data, hence clarifying the ostensible existing contradictions.

  6. AC Electrowetting of Polymer Aqueous Drops on Parallel Electrodes

    Science.gov (United States)

    Zhang, Lu; Chetwani, Nishant; Chang, Hsueh-Chia; Zhu, Yingxi Elaine

    2009-03-01

    We have recently observed the strong field dependence of AC-electrowetting of simple electrolyte aqueous drops on parallel gold electrodes, yet the detailed dynamic process of AC-field induced surface wetting remains unclear. In this work, we use fluorescence labeled DNA aqueous solution as a model system to directly visualize the wetting process of aqueous drops under varied AC electric fields by using combined fluorescence microscopy and contact angle goniometer. The electrowetting behavior of DNA aqueous drops is observed at AC-field frequency greater than the reciprocal of the RC time scale for electrode screening. And the onset of AC electrowetting is accompanied by the observed oscillation in drop contour shape and contact line. In addition, the ejection of nanodrops from the parent aqueous drop is observed when the threshold AC-field amplitude is exceeded. A scaling theory based on electrode interfacial screening is developed to quantify the AC-electrowetting behavior with the dependence of AC-field frequency, strength and medium conductivity.

  7. Leidenfrost drops on a heated liquid pool

    Science.gov (United States)

    Maquet, L.; Sobac, B.; Darbois-Texier, B.; Duchesne, A.; Brandenbourger, M.; Rednikov, A.; Colinet, P.; Dorbolo, S.

    2016-09-01

    We show that a volatile liquid drop placed at the surface of a nonvolatile liquid pool warmer than the boiling point of the drop can be held in a Leidenfrost state even for vanishingly small superheats. Such an observation points to the importance of the substrate roughness, negligible in the case considered here, in determining the threshold Leidenfrost temperature. A theoretical model based on the one proposed by Sobac et al. [Phys. Rev. E 90, 053011 (2014), 10.1103/PhysRevE.90.053011] is developed in order to rationalize the experimental data. The shapes of the drop and of the liquid substrate are analyzed. The model notably provides scalings for the vapor film thickness profile. For small drops, these scalings appear to be identical to the case of a Leidenfrost drop on a solid substrate. For large drops, in contrast, they are different, and no evidence of chimney formation has been observed either experimentally or theoretically in the range of drop sizes considered in this study. Concerning the evaporation dynamics, the radius is shown to decrease linearly with time whatever the drop size, which differs from the case of a Leidenfrost drop on a solid substrate. For high superheats, the characteristic lifetime of the drops versus the superheat follows a scaling law that is derived from the model, but, at low superheats, it deviates from this scaling by rather saturating.

  8. Cutting a drop of water pinned by wire loops using a superhydrophobic surface and knife.

    Directory of Open Access Journals (Sweden)

    Ryan Yanashima

    Full Text Available A water drop on a superhydrophobic surface that is pinned by wire loops can be reproducibly cut without formation of satellite droplets. Drops placed on low-density polyethylene surfaces and Teflon-coated glass slides were cut with superhydrophobic knives of low-density polyethylene and treated copper or zinc sheets, respectively. Distortion of drop shape by the superhydrophobic knife enables a clean break. The driving force for droplet formation arises from the lower surface free energy for two separate drops, and it is modeled as a 2-D system. An estimate of the free energy change serves to guide when droplets will form based on the variation of drop volume, loop spacing and knife depth. Combining the cutting process with an electrofocusing driving force could enable a reproducible biomolecular separation without troubling satellite drop formation.

  9. Star-shaped oscillations of Leidenfrost drops

    Science.gov (United States)

    Ma, Xiaolei; Liétor-Santos, Juan-José; Burton, Justin C.

    2017-03-01

    We experimentally investigate the self-sustained, star-shaped oscillations of Leidenfrost drops. The drops levitate on a cushion of evaporated vapor over a heated, curved surface. We observe modes with n =2 -13 lobes around the drop periphery. We find that the wavelength of the oscillations depends only on the capillary length of the liquid and is independent of the drop radius and substrate temperature. However, the number of observed modes depends sensitively on the liquid viscosity. The dominant frequency of pressure variations in the vapor layer is approximately twice the drop oscillation frequency, consistent with a parametric forcing mechanism. Our results show that the star-shaped oscillations are driven by capillary waves of a characteristic wavelength beneath the drop and that the waves are generated by a large shear stress at the liquid-vapor interface.

  10. Sepsis from dropped clips at laparoscopic cholecystectomy

    Energy Technology Data Exchange (ETDEWEB)

    Hussain, Sarwat E-mail: sarwathussain@hotmail.com

    2001-12-01

    We report seven patients in whom five dropped surgical clips and two gallstones were visualized in the peritoneal cavity, on radiological studies. In two, subphrenic abscesses and empyemas developed as a result of dropped clips into the peritoneal cavity during or following laparoscopic cholecystectomy. In one of these two, a clip was removed surgically from the site of an abscess. In two other patients dropped gallstones, and in three, dropped clips led to no complications. These were seen incidentally on studies done for other indications. Abdominal abscess secondary to dropped gallstones is a well-recognized complication of laparoscopic cholecystectomy (LC). We conclude that even though dropped surgical clips usually do not cause problems, they should be considered as a risk additional to other well-known causes of post-LC abdominal sepsis.

  11. Sepsis from dropped clips at laparoscopic cholecystectomy

    International Nuclear Information System (INIS)

    Hussain, Sarwat

    2001-01-01

    We report seven patients in whom five dropped surgical clips and two gallstones were visualized in the peritoneal cavity, on radiological studies. In two, subphrenic abscesses and empyemas developed as a result of dropped clips into the peritoneal cavity during or following laparoscopic cholecystectomy. In one of these two, a clip was removed surgically from the site of an abscess. In two other patients dropped gallstones, and in three, dropped clips led to no complications. These were seen incidentally on studies done for other indications. Abdominal abscess secondary to dropped gallstones is a well-recognized complication of laparoscopic cholecystectomy (LC). We conclude that even though dropped surgical clips usually do not cause problems, they should be considered as a risk additional to other well-known causes of post-LC abdominal sepsis

  12. Hydrothermal waves in evaporating sessile drops

    OpenAIRE

    Brutin, D.; Rigollet, F.; Niliot, C. Le

    2009-01-01

    Drop evaporation is a simple phenomena but still unclear concerning the mechanisms of evaporation. A common agreement of the scientific community based on experimental and numerical work evidences that most of the evaporation occurs at the triple line. However, the rate of evaporation is still empirically predicted due to the lack of knowledge on the convection cells which develop inside the drop under evaporation. The evaporation of sessile drop is more complicated than it appears due to the...

  13. Fully Automatic In-Syringe Magnetic Stirring-Assisted Dispersive Liquid–Liquid Microextraction Hyphenated to High-Temperature Torch Integrated Sample Introduction System-Inductively Coupled Plasma Spectrometer with Direct Injection of the Organic Phase

    OpenAIRE

    Sánchez, Raquel; Horstkotte, Burkhard; Fikarová, Kateřina; Sklenářová, Hana; Maestre, Salvador E.; Miró, Manuel; Todolí Torró, José Luis

    2017-01-01

    A proof of concept study involving the online coupling of automatic dispersive liquid–liquid microextraction (DLLME) to inductively coupled plasma optical emission spectrometry (ICP OES) with direct introduction and analysis of the organic extract is herein reported for the first time. The flow-based analyzer features a lab-in-syringe (LIS) setup with an integrated stirring system, a Meinhard nebulizer in combination with a heated single-pass spray chamber, and a rotary injection valve, used ...

  14. Soft drop jet mass measurement

    CERN Document Server

    Roloff, Jennifer Kathryn; The ATLAS collaboration

    2018-01-01

    Calculations of jet substructure observables that are accurate beyond leading-logarithm accuracy have recently become available. Such observables are significant not only for probing the collinear regime of QCD that is largely unexplored at a hadron collider, but also for improving the understanding of jet substructure properties that are used in many studies at the Large Hadron Collider. This poster documents a measurement of the first jet substructure quantity at a hadron collider to be calculated at next-to-next-to-leading-logarithm accuracy. The normalized, differential cross-section is measured as a function of log( ρ^2), where ρ is the ratio of the soft-drop mass to the ungroomed jet transverse momentum. This quantity is measured in dijet events from 32.9 ifb of sqrt(s) = 13 TeV proton-proton collisions recorded by the ATLAS detector. The data are unfolded to correct for detector effects and compared to precise QCD calculations and leading-logarithm particle-level Monte Carlo simulations.

  15. Are the Stress Drops of Small Earthquakes Good Predictors of the Stress Drops of Larger Earthquakes?

    Science.gov (United States)

    Hardebeck, J.

    2017-12-01

    Uncertainty in PSHA could be reduced through better estimates of stress drop for possible future large earthquakes. Studies of small earthquakes find spatial variability in stress drop; if large earthquakes have similar spatial patterns, their stress drops may be better predicted using the stress drops of small local events. This regionalization implies the variance with respect to the local mean stress drop may be smaller than the variance with respect to the global mean. I test this idea using the Shearer et al. (2006) stress drop catalog for M1.5-3.1 events in southern California. I apply quality control (Hauksson, 2015) and remove near-field aftershocks (Wooddell & Abrahamson, 2014). The standard deviation of the distribution of the log10 stress drop is reduced from 0.45 (factor of 3) to 0.31 (factor of 2) by normalizing each event's stress drop by the local mean. I explore whether a similar variance reduction is possible when using the Shearer catalog to predict stress drops of larger southern California events. For catalogs of moderate-sized events (e.g. Kanamori, 1993; Mayeda & Walter, 1996; Boyd, 2017), normalizing by the Shearer catalog's local mean stress drop does not reduce the standard deviation compared to the unmodified stress drops. I compile stress drops of larger events from the literature, and identify 15 M5.5-7.5 earthquakes with at least three estimates. Because of the wide range of stress drop estimates for each event, and the different techniques and assumptions, it is difficult to assign a single stress drop value to each event. Instead, I compare the distributions of stress drop estimates for pairs of events, and test whether the means of the distributions are statistically significantly different. The events divide into 3 categories: low, medium, and high stress drop, with significant differences in mean stress drop between events in the low and the high stress drop categories. I test whether the spatial patterns of the Shearer catalog

  16. Air-assisted liquid-liquid microextraction used for the rapid determination of organophosphorus pesticides in juice samples.

    Science.gov (United States)

    You, Xiangwei; Xing, Zhuokan; Liu, Fengmao; Jiang, Naiwen

    2013-10-11

    A novel and simple air-assisted liquid-liquid microextraction (AALLME) is introduced to analyze the organophosphorus pesticide (OPP) residues in fruit juice samples, using the gas chromatography-flame photometric detection (GC-FPD). In this method, fine extraction solvent drops are rapidly formed and dispersed into the aqueous samples, by using a syringe to withdraw and push-out the mixture of aqueous sample solution and extraction solvent several times. The parameters affecting the extraction efficiency were investigated including the type and volume of the extraction solvent, salt addition, extraction times, and pH. Under optimized conditions, the method showed good linearities with the correlation coefficients (γ) higher than 0.9988, and the sensitivity with the limits of detection (LODs) between 0.02μgL(-1) and 0.6μgL(-1). The method was applied to determine the OPP residues in juice samples and the recoveries were ranged from 79% to 113% with relative standard deviations (RSDs) of 0.4-9.9%. The feasibility of the method in real samples was proved. Copyright © 2013 Elsevier B.V. All rights reserved.

  17. Many Drops Make a Lake

    Directory of Open Access Journals (Sweden)

    Chaitanya S. Mudgal

    2014-03-01

    greater knowledge, better skills and disseminate this knowledge through this journal to influence as many physicians and their patients as possible. They have taken the knowledge of their teachers, recognized their giants and are now poised to see further than ever before. My grandmother often used to quote to me a proverb from India, which when translated literally means “Many drops make a lake”. I cannot help but be amazed by the striking similarities between the words of Newton and this Indian saying. Therefore, while it may seem intuitive, I think it must be stated that it is vital for the betterment of all our patients that we recognize our own personal lakes to put our drops of knowledge into. More important is that we recognize that it is incumbent upon each and every one of us to contribute to our collective lakes of knowledge such as ABJS. And finally and perhaps most importantly we need to be utterly cognizant of never letting such lakes of knowledge run dry.... ever.

  18. Identification of volatile compounds in soybean at various developmental stages using solid phase microextraction.

    Science.gov (United States)

    Boué, Stephen M; Shih, Betty Y; Carter-Wientjes, Carol H; Cleveland, Thomas E

    2003-08-13

    Soybean (Glycine max) seed volatiles were analyzed using a solid phase microextraction (SPME) method combined with gas chromatography-mass spectrometry (GC-MS). Thirty volatile compounds already reported for soybean were recovered, and an additional 19 compounds not previously reported were identified or tentatively identified. The SPME method was utilized to compare the volatile profile of soybean seed at three distinct stages of development. Most of the newly reported compounds in soybean seed were aldehydes and ketones. During early periods of development at maturity stage R6, several volatiles were present at relatively high concentrations, including 3-hexanone, (E)-2-hexenal, 1-hexanol, and 3-octanone. At maturity stage R7 and R8, decreased amounts of 3-hexanone, (E)-2-hexenal, 1-hexanol, and 3-octanone were observed. At maturity stage R8 hexanal, (E)-2-heptenal, (E)-2-octenal, ethanol, 1-hexanol, and 1-octen-3-ol were detected at relatively high concentrations. SPME offers the ability to differentiate between the three soybean developmental stages that yield both fundamental and practical information.

  19. Drop test facility available to private industry

    International Nuclear Information System (INIS)

    Shappert, L.B.; Box, W.D.

    1983-01-01

    In 1978, a virtually unyielding drop test impact pad was constructed at Oak Ridge National Laboratory's (ORNL's) Tower Shielding Facility (TSF) for the testing of heavy shipping containers designed for transporting radioactive materials. Because of the facility's unique capability for drop-testing large, massive shipping packages, it has been identified as a facility which can be made available for non-DOE users

  20. Total Site Heat Integration Considering Pressure Drops

    Directory of Open Access Journals (Sweden)

    Kew Hong Chew

    2015-02-01

    Full Text Available Pressure drop is an important consideration in Total Site Heat Integration (TSHI. This is due to the typically large distances between the different plants and the flow across plant elevations and equipment, including heat exchangers. Failure to consider pressure drop during utility targeting and heat exchanger network (HEN synthesis may, at best, lead to optimistic energy targets, and at worst, an inoperable system if the pumps or compressors cannot overcome the actual pressure drop. Most studies have addressed the pressure drop factor in terms of pumping cost, forbidden matches or allowable pressure drop constraints in the optimisation of HEN. This study looks at the implication of pressure drop in the context of a Total Site. The graphical Pinch-based TSHI methodology is extended to consider the pressure drop factor during the minimum energy requirement (MER targeting stage. The improved methodology provides a more realistic estimation of the MER targets and valuable insights for the implementation of the TSHI design. In the case study, when pressure drop in the steam distribution networks is considered, the heating and cooling duties increase by 14.5% and 4.5%.

  1. Microwave-assisted headspace single-drop microextration of chlorobenzenes from water samples

    Energy Technology Data Exchange (ETDEWEB)

    Vidal, Lorena [Departamento de Quimica Analitica, Nutricion y Bromatologia, Universidad de Alicante, P.O. Box 99, E-03080 Alicante (Spain); Domini, Claudia E. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Universidad de Alicante, P.O. Box 99, E-03080 Alicante (Spain); Grane, Nuria [Departamento de Quimica Analitica, Nutricion y Bromatologia, Universidad de Alicante, P.O. Box 99, E-03080 Alicante (Spain); Psillakis, Elefteria [Department of Environmental Engineering, Technical University of Crete, Polytechneioupolis, GR-73100 Chania, Crete (Greece); Canals, Antonio [Departamento de Quimica Analitica, Nutricion y Bromatologia, Universidad de Alicante, P.O. Box 99, E-03080 Alicante (Spain)]. E-mail: a.canals@ua.es

    2007-05-29

    A one-step and in-situ sample preparation method used for quantifying chlorobenzene compounds in water samples has been developed, coupling microwave and headspace single-drop microextraction (MW-HS-SDME). The chlorobenzenes in water samples were extracted directly onto an ionic liquid single-drop in headspace mode under the aid of microwave radiation. For optimization, a Plackett-Burman screening design was initially used, followed by a mixed-level factorial design. The factors considered were: drop volume, aqueous sample volume, stirring speed, ionic strength, extraction time, ionic liquid type, microwave power and length of the Y-shaped glass-tube. The optimum experimental conditions found from this statistical evaluation were: a 5 {mu}L microdrop of 1-hexyl-3-methylimidazolium hexafluorophosphate exposed for 20 min to the headspace of a 30 mL aqueous sample, irradiated by microwaves at 200 W and placed in a 50 mL spherical flask connected to a 25 cm Y-shaped glass-tube. Under the optimised experimental conditions, the response of a high performance liquid chromatographic system was found to be linear over the range studied and with correlation coefficients ranging between 0.9995 and 0.9999. The method showed a good level of repeatability, with relative standard deviations varying between 2.3 and 8.3% (n = 5). Detection limits were found in the low {mu}g L{sup -1} range varying between 0.016 and 0.039 {mu}g L{sup -1}. Overall, the performance of the proposed method demonstrated the favourable effect of microwave sample irradiation upon HS-SDME. Finally, recovery studies from different types of environmental water samples revealed that matrix had little effect upon extraction.

  2. Microwave-assisted headspace single-drop microextration of chlorobenzenes from water samples

    International Nuclear Information System (INIS)

    Vidal, Lorena; Domini, Claudia E.; Grane, Nuria; Psillakis, Elefteria; Canals, Antonio

    2007-01-01

    A one-step and in-situ sample preparation method used for quantifying chlorobenzene compounds in water samples has been developed, coupling microwave and headspace single-drop microextraction (MW-HS-SDME). The chlorobenzenes in water samples were extracted directly onto an ionic liquid single-drop in headspace mode under the aid of microwave radiation. For optimization, a Plackett-Burman screening design was initially used, followed by a mixed-level factorial design. The factors considered were: drop volume, aqueous sample volume, stirring speed, ionic strength, extraction time, ionic liquid type, microwave power and length of the Y-shaped glass-tube. The optimum experimental conditions found from this statistical evaluation were: a 5 μL microdrop of 1-hexyl-3-methylimidazolium hexafluorophosphate exposed for 20 min to the headspace of a 30 mL aqueous sample, irradiated by microwaves at 200 W and placed in a 50 mL spherical flask connected to a 25 cm Y-shaped glass-tube. Under the optimised experimental conditions, the response of a high performance liquid chromatographic system was found to be linear over the range studied and with correlation coefficients ranging between 0.9995 and 0.9999. The method showed a good level of repeatability, with relative standard deviations varying between 2.3 and 8.3% (n = 5). Detection limits were found in the low μg L -1 range varying between 0.016 and 0.039 μg L -1 . Overall, the performance of the proposed method demonstrated the favourable effect of microwave sample irradiation upon HS-SDME. Finally, recovery studies from different types of environmental water samples revealed that matrix had little effect upon extraction

  3. Drop dispensing in a viscous outer liquid

    Directory of Open Access Journals (Sweden)

    Claudiu PATRASCU

    2017-12-01

    Full Text Available The formation and detachment of Newtonian drops in viscous external liquids is investigated. A global analysis of two necking processes is presented in order to highlight the behavior of such thinning phenomena, when controlled either by inertia or by viscous effects. Moving detached droplets in an immiscible outer liquid were studied in terms of velocity and drop-travel distance. Theoretical predictions are proposed and compared with experimental data for the volume of the drop and for the subsequent dynamics that follow after detachment. Our investigations point out that the drop rapidly achieves constant velocity, the value of it being in a satisfactory agreement with the model. Both the influence of the flow rate and that of the material properties on drop volume are pursued.

  4. Breakfast patterns of frozen impacted drops

    Science.gov (United States)

    Thievenaz, Virgile; Josserand, Christophe; Seon, Thomas

    2017-11-01

    We investigate experimentally the solidification of a water drop during its impact on a sub-zero cooled metallic plate. As the drop impacts the substrate, a first thin layer of ice builds-up in the briefest moment. Afterwards, the competition between the liquid solidification and its retraction on this ice layer leads to a variety of frozen drop patterns. Typically, with a change of temperature the drop can freeze into a fried egg or a doughnut shape. These frozen motifs experience different sizes and can even disappear so only the thin pancake remains. These patterns have been explored through a range of parameters such as : plate temperature, thermal properties, drop size and impact velocity. Phase-diagrams show the range and the transition temperatures between the different patterns as a function of those parameters. The experimental results are discussed using a scaling law approach, allowing basic understanding of the underlying physics.

  5. Wetting and evaporation of binary mixture drops.

    Science.gov (United States)

    Sefiane, Khellil; David, Samuel; Shanahan, Martin E R

    2008-09-11

    Experimental results on the wetting behavior of water, methanol, and binary mixture sessile drops on a smooth, polymer-coated substrate are reported. The wetting behavior of evaporating water/methanol drops was also studied in a water-saturated environment. Drop parameters (contact angle, shape, and volume) were monitored in time. The effects of the initial relative concentrations on subsequent evaporation and wetting dynamics were investigated. Physical mechanisms responsible for the various types of wetting behavior during different stages are proposed and discussed. Competition between evaporation and hydrodynamic flow are evoked. Using an environment saturated with water vapor allowed further exploration of the controlling mechanisms and underlying processes. Wetting stages attributed to differential evaporation of methanol were identified. Methanol, the more volatile component, evaporates predominantly in the initial stage. The data, however, suggest that a small proportion of methanol remained in the drop after the first stage of evaporation. This residual methanol within the drop seems to influence subsequent wetting behavior strongly.

  6. Comparison of dispersive liquid-liquid microextraction and hollow fiber liquid-liquid-liquid microextraction for the determination of fentanyl, alfentanil, and sufentanil in water and biological fluids by high-performance liquid chromatography.

    Science.gov (United States)

    Saraji, Mohammad; Khalili Boroujeni, Malihe; Hajialiakbari Bidgoli, Ali Akbar

    2011-06-01

    Dispersive liquid-liquid microextraction (DLLME) and hollow fiber liquid-liquid-liquid microextraction (HF-LLLME) combined with HPLC-DAD have been applied for the determination of three narcotic drugs (alfentanil, fentanyl, and sufentanil) in biological samples (human plasma and urine). Different DLLME parameters influencing the extraction efficiency such as type and volume of the extraction solvent and the disperser solvent, concentration of NaOH, and salt addition were investigated. In the HF-LLLME, the effects of important parameters including organic solvent type, concentration of NaOH as donor solution, concentration of H(2)SO(4) as acceptor phase, salt addition, stirring rate, temperature, and extraction time were investigated and optimized. The results showed that both extraction methods exhibited good linearity, precision, enrichment factor, and detection limit. Under optimal condition, the limits of detection ranged from 0.4 to 1.9 μg/L and from 1.1 to 2.3 μg/L for DLLME and HF-LLLME, respectively. For DLLME, the intra- and inter-day precisions were 1.7-6.4% and 14.2-15.9%, respectively; and for HF-LLLME were 0.7-5.2% and 3.3-10.1%, respectively. The enrichment factors were from 275 to 325 and 190 to 237 for DLLME and HF-LLLME, respectively. The applicability of the proposed methods was investigated by analyzing biological samples. For analysis of human plasma and urine samples, HF-LLLME showed higher precision, more effective sample clean-up, higher extraction efficiency, lower organic solvent consumption than DLLME.

  7. Initial Electrospreading of Aqueous Electrolyte Drops

    Science.gov (United States)

    Chen, Longquan; Li, Chunli; van der Vegt, Nico F. A.; Auernhammer, Günter K.; Bonaccurso, Elmar

    2013-01-01

    The early spreading of a liquid drop on a solid surface driven by inertial, capillary, and electrostatic forces is of fundamental interest, since most commonly used surfaces are (naturally) charged. We studied the effect of applying an electric potential between a drop and a surface on the early spreading of aqueous electrolyte drops. We found that spreading dynamics not only depended on the potential, but also on the electrolyte concentration. Based on molecular dynamics simulations of the ion distribution in spreading nanodrops under an applied potential, we propose a simple model to explain the relation between applied potential, electrolyte concentration, and early spreading dynamics.

  8. Carbon nanotubes reinforced hollow fiber solid phase microextraction for the determination of strychnine and brucine in urine.

    Science.gov (United States)

    Song, Xin-Yue; Shi, Yan-Ping; Chen, Juan

    2013-11-15

    A mixed matrix membrane (MMM), based on carbon nanotubes (CNTs) and hollow fiber (HF), was prepared and combined with solid phase microextraction (SPME) mode to determine strychnine and brucine in urine. This MMM was prepared by dispersing CNTs in water via surfactant assistance, and then immobilizing CNTs into the pores of HF by capillary forces and sonification. The prepared carbon nanotubes reinforced hollow fiber (CNTs-HF) was subsequently wetted by a few microliters of organic solvent (1-octanol), and then applied to extract the target analytes in direct immersion sampling mode. After extraction, analytes were desorbed via ultrasonic-assisted effect, and then detected via high-performance liquid chromatography (HPLC). To achieve the highest extraction efficiency, main extraction parameters such as the type and amount of surfactant, the diameter and doping level of CNTs, extraction time, desorption condition, pH value, stirring rate and volume of the donor phase were optimized. Under the optimum extraction conditions, the method showed good linearity ranges with correlation coefficients higher than 0.9990, good repeatability and batch-to-batch reproducibility with relative standard deviations (RSDs) less than 6% and 5% for strychnine and brucine, respectively, and low limits of detection (0.7 and 0.9 µg L(-1) for strychnine and brucine, respectively). The recoveries were in the range of 83.81-116.14% at three spiked levels. The developed method was successfully applied to real urine sample with mean relative recoveries of 94.28% and 91.30% for strychnine and brucine, respectively. The developed method shows comparable results against reference methods and is a simple, green, and cost-effective microextraction technique. © 2013 Elsevier B.V. All rights reserved.

  9. Evaluation of needle trap micro-extraction and automatic alveolar sampling for point-of-care breath analysis.

    Science.gov (United States)

    Trefz, Phillip; Rösner, Lisa; Hein, Dietmar; Schubert, Jochen K; Miekisch, Wolfram

    2013-04-01

    Needle trap devices (NTDs) have shown many advantages such as improved detection limits, reduced sampling time and volume, improved stability, and reproducibility if compared with other techniques used in breath analysis such as solid-phase extraction and solid-phase micro-extraction. Effects of sampling flow (2-30 ml/min) and volume (10-100 ml) were investigated in dry gas standards containing hydrocarbons, aldehydes, and aromatic compounds and in humid breath samples. NTDs contained (single-bed) polymer packing and (triple-bed) combinations of divinylbenzene/Carbopack X/Carboxen 1000. Substances were desorbed from the NTDs by means of thermal expansion and analyzed by gas chromatography-mass spectrometry. An automated CO2-controlled sampling device for direct alveolar sampling at the point-of-care was developed and tested in pilot experiments. Adsorption efficiency for small volatile organic compounds decreased and breakthrough increased when sampling was done with polymer needles from a water-saturated matrix (breath) instead from dry gas. Humidity did not affect analysis with triple-bed NTDs. These NTDs showed only small dependencies on sampling flow and low breakthrough from 1-5 %. The new sampling device was able to control crucial parameters such as sampling flow and volume. With triple-bed NTDs, substance amounts increased linearly with increasing sample volume when alveolar breath was pre-concentrated automatically. When compared with manual sampling, automatic sampling showed comparable or better results. Thorough control of sampling and adequate choice of adsorption material is mandatory for application of needle trap micro-extraction in vivo. The new CO2-controlled sampling device allows direct alveolar sampling at the point-of-care without the need of any additional sampling, storage, or pre-concentration steps.

  10. Low-voltage electrochemically stimulated stir membrane liquid-liquid microextraction as a novel technique for the determination of methadone.

    Science.gov (United States)

    Ara, Katayoun Mahdavi; Raofie, Farhad

    2017-06-01

    In the present work, for the first time, a new portable setup was designed, developed and presented for the extraction of methadone, as a basic drug model from biological fluid samples using a low-voltage electrically stimulated stir membrane liquid-liquid microextraction technique (LV-ESSM-LLME), followed by high-performance liquid chromatography with ultraviolet detection. This new approach combines the advantages of stir membrane liquid-liquid microextraction and electrokinetic migration in the same unit under soft electrochemical conditions in a portable device, allowing for the isolation and preconcentration of the target analyte in a simple and efficient manner under three-phase mode. To investigate the influence of external stirring and the application of electrical potential as the driving force, a comparative study of all variables involved in the extraction process was carried out using the low-voltage electromembrane extraction (LV-EME) and LV-ESSM-LLME methods. Under soft electrokinetic migration conditions, methadone was transported from an acidic sample solution (pH 4.0), through the NPOE immobilized in the pores of the porous polypropylene sheet membrane, and into 25µL of 10mmolL -1 HCl acceptor solution with a stirring rate of 1000rpm and 700rpm after 15min and 20min for LV-ESSM-LLME and LV-EME, respectively. Under the optimized conditions, preconcentration factors in the range of 17-24 and 21.5-29 for LV-EME and LV-ESSM-LLME, respectively, were considered, and satisfactory repeatability (4.5<[RSD]<7.5) was obtained in different matrices. The obtained relative recoveries of the target analyte were in the range of 87-94% and 93-101% for LV-EME and LV-ESSM-LLME, respectively, which indicated the excellent capability of the developed methods to extract methadone from complex matrices. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Micro-splashing by drop impacts

    KAUST Repository

    Thoroddsen, Sigurdur T.

    2012-07-18

    We use ultra-high-speed video imaging to observe directly the earliest onset of prompt splashing when a drop impacts onto a smooth solid surface. We capture the start of the ejecta sheet travelling along the solid substrate and show how it breaks up immediately upon emergence from the underneath the drop. The resulting micro-droplets are much smaller and faster than previously reported and may have gone unobserved owing to their very small size and rapid ejection velocities, which approach 100 m s-1, for typical impact conditions of large rain drops. We propose a phenomenological mechanism which predicts the velocity and size distribution of the resulting microdroplets. We also observe azimuthal undulations which may help promote the earliest breakup of the ejecta. This instability occurs in the cusp in the free surface where the drop surface meets the radially ejected liquid sheet. © 2012 Cambridge University Press.

  12. Development of Active Learning Curriculum for CASPER's Microgravity Drop Tower

    Science.gov (United States)

    Carmona-Reyes, Jorge; Wang, Li; York, Judy; Matthews, Lorin; Laufer, Rene; Cook, Mike; Schmoke, Jimmy; Hyde, Truell

    2016-10-01

    As CASPER's new drop tower comes on line, plans for correlated educational research curricula are underway. CASPER's educational research team is working on developing curricula specific to the CASPER drop tower, modeled on a contest currently in use by (BEST) Robotics Inc. within central Texas independent school districts. The curricula integrates age specific use of computer programming software packages such as ``Scratch'' with industry standard communication protocols and augmented reality applications. Content is constructed around an earth and space science framework, covering subjects such as stars and galaxies, matter and energy, fusion and fission at a middle school level. CASPER faculty are partnering with the Region 12 Service Center; this combination provides a wide range of expertise that includes professional development, pedagogical methods, computational thinking in addition to microgravity and space science research expertise. The details of this work will be presented and samples of the manner in which it is impacting the CASPER research and educational outreach partnership will be discussed.

  13. Blood drop patterns: Formation and applications.

    Science.gov (United States)

    Chen, Ruoyang; Zhang, Liyuan; Zang, Duyang; Shen, Wei

    2016-05-01

    The drying of a drop of blood or plasma on a solid substrate leads to the formation of interesting and complex patterns. Inter- and intra-cellular and macromolecular interactions in the drying plasma or blood drop are responsible for the final morphologies of the dried patterns. Changes in these cellular and macromolecular components in blood caused by diseases have been suspected to cause changes in the dried drop patterns of plasma and whole blood, which could be used as simple diagnostic tools to identify the health of humans and livestock. However, complex physicochemical driving forces involved in the pattern formation are not fully understood. This review focuses on the scientific development in microscopic observations and pattern interpretation of dried plasma and whole blood samples, as well as the diagnostic applications of pattern analysis. Dried drop patterns of plasma consist of intricate visible cracks in the outer region and fine structures in the central region, which are mainly influenced by the presence and concentration of inorganic salts and proteins during drying. The shrinkage of macromolecular gel and its adhesion to the substrate surface have been thought to be responsible for the formation of the cracks. Dried drop patterns of whole blood have three characteristic zones; their formation as functions of drying time has been reported in the literature. Some research works have applied engineering treatment to the evaporation process of whole blood samples. The sensitivities of the resultant patterns to the relative humidity of the environment, the wettability of the substrates, and the size of the drop have been reported. These research works shed light on the mechanisms of spreading, evaporation, gelation, and crack formation of the blood drops on solid substrates, as well as on the potential applications of dried drop patterns of plasma and whole blood in diagnosis. Crown Copyright © 2016. Published by Elsevier B.V. All rights reserved.

  14. Pressure drop in flashing flow through obstructions

    International Nuclear Information System (INIS)

    Weinle, M.E.; Johnston, B.S.

    1985-01-01

    An experiment was designed to investigate the pressure drop for flashing flow across obstructions of different geometries at various flow rates. Tests were run using two different orifices to determine if the two-phase pressure drop could be characterized by the single phase loss coefficient and the general behavior of the two-phase multiplier. For the geometries studied, it was possible to correlate the multiplier in a geometry-independent fashion

  15. Determination of triazine herbicides in juice samples by microwave-assisted ionic liquid/ionic liquid dispersive liquid-liquid microextraction coupled with high-performance liquid chromatography.

    Science.gov (United States)

    Su, Rui; Li, Dan; Wu, Lijie; Han, Jing; Lian, Wenhui; Wang, Keren; Yang, Hongmei

    2017-07-01

    A novel microextraction method, termed microwave-assisted ionic liquid/ionic liquid dispersive liquid-liquid microextraction, has been developed for the rapid enrichment and analysis of triazine herbicides in fruit juice samples by high-performance liquid chromatography. Instead of using hazardous organic solvents, two kinds of ionic liquids, a hydrophobic ionic liquid (1-hexyl-3-methylimidazolium hexafluorophosphate) and a hydrophilic ionic liquid (1-butyl-3-methylimidazolium tetrafluoroborate), were used as the extraction solvent and dispersion agent, respectively, in this method. The extraction procedure was induced by the formation of cloudy solution, which was composed of fine drops of 1-hexyl-3-methylimidazolium hexafluorophosphate dispersed entirely into sample solution with the help of 1-butyl-3-methylimidazolium tetrafluoroborate. In addition, an ion-pairing agent (NH 4 PF 6 ) was introduced to improve recoveries of the ionic liquid phase. Several experimental parameters that might affect the extraction efficiency were investigated. Under the optimum experimental conditions, the linearity for determining the analytes was in the range of 5.00-250.00 μg/L, with the correlation coefficients of 0.9982-0.9997. The practical application of this effective and green method is demonstrated by the successful analysis of triazine herbicides in four juice samples, with satisfactory recoveries (76.7-105.7%) and relative standard deviations (lower than 6.6%). In general, this method is fast, effective, and robust to determine triazine herbicides in juice samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Headspace solid-phase microextraction for wine volatile analysis.

    Science.gov (United States)

    Azzi-Achkouty, Samar; Estephan, Nathalie; Ouaini, Naïm; Rutledge, Douglas N

    2017-07-03

    The most commonly used technique to prepare samples for the analysis of wine volatile is the headspace solid-phase microextraction (HS-SPME). This method has gained popularity in last few years, as it is a unique solventless preparation technique. In this paper, a summary of recently published studies using HS-SPME for the analysis of wine aromas, with special emphasis on the method developed, has been compiled. Several papers are discussed in detail, mainly with respect to the SPME conditions used. A brief summary of the reviews related to HS-SPME analysis is given and discussed. Several parameters affecting the HS-SPME, such as the salt concentration and the agitation conditions, are used in the same way as used in several papers. The HS-SPME extraction proved to be sufficiently sensitive to satisfy legislative requirements related to low detection and quantification limits as well as method accuracy and precision requirements. However, in order to achieve the best performance and precision, the protocol needs to be optimized for each case. The effect of different parameters must be well characterized to ensure correct extraction and desorption to ensure the transfer of extracted compounds into the analytical system. The operating parameters, such as time, temperature, and agitation, must then be kept constant for all the samples.

  17. Fully Automatic In-Syringe Magnetic Stirring-Assisted Dispersive Liquid-Liquid Microextraction Hyphenated to High-Temperature Torch Integrated Sample Introduction System-Inductively Coupled Plasma Spectrometer with Direct Injection of the Organic Phase.

    Science.gov (United States)

    Sánchez, Raquel; Horstkotte, Burkhard; Fikarová, Kateřina; Sklenářová, Hana; Maestre, Salvador; Miró, Manuel; Todolí, Jose-Luis

    2017-03-21

    A proof of concept study involving the online coupling of automatic dispersive liquid-liquid microextraction (DLLME) to inductively coupled plasma optical emission spectrometry (ICP OES) with direct introduction and analysis of the organic extract is herein reported for the first time. The flow-based analyzer features a lab-in-syringe (LIS) setup with an integrated stirring system, a Meinhard nebulizer in combination with a heated single-pass spray chamber, and a rotary injection valve, used as an online interface between the microextraction system and the detection instrument. Air-segmented flow was used for delivery of a fraction of the nonwater miscible extraction phase, 12 μL of xylene, to the nebulizer. All sample preparative steps including magnetic stirring assisted DLLME were carried out inside the syringe void volume as a size-adaptable yet sealed mixing and extraction chamber. Determination of trace level concentrations of cadmium, copper, lead, and silver as model analytes has been demonstrated by microextraction as diethyldithiophosphate (DDTP) complexes. The automatic LIS-DLLME method features quantitative metal extraction, even in troublesome sample matrixes, such as seawater, salt, and fruit juices, with relative recoveries within the range of 94-103%, 93-100%, and 92-99%, respectively. Furthermore, no statistically significant differences at the 0.05 significance level were found between concentration values experimentally obtained and the certified values of two serum standard reference materials.

  18. The Drop Tower Bremen -Experiment Operation

    Science.gov (United States)

    Könemann, Thorben; von Kampen, Peter; Rath, Hans J.

    The idea behind the drop tower facility of the Center of Applied Space Technology and Micro-gravity (ZARM) in Bremen is to provide an inimitable technical opportunity of a daily access to short-term weightlessness on earth. In this way ZARM`s european unique ground-based microgravity laboratory displays an excellent economic alternative for research in space-related conditions at low costs comparable to orbital platforms. Many national and international ex-perimentalists motivated by these prospects decide to benefit from the high-quality and easy accessible microgravity environment only provided by the Drop Tower Bremen. Corresponding experiments in reduced gravity could open new perspectives of investigation methods and give scientists an impressive potential for a future technology and multidisciplinary applications on different research fields like Fundamental Physics, Astrophysics, Fluid Dynamics, Combus-tion, Material Science, Chemistry and Biology. Generally, realizing microgravity experiments at ZARM`s drop tower facility meet new requirements of the experimental hardware and may lead to some technical constraints in the setups. In any case the ZARM Drop Tower Operation and Service Company (ZARM FAB mbH) maintaining the drop tower facility is prepared to as-sist experimentalists by offering own air-conditioned laboratories, clean rooms, workshops and consulting engineers, as well as scientific personal. Furthermore, ZARM`s on-site apartment can be used for accommodations during the experiment campaigns. In terms of approaching drop tower experimenting, consulting of experimentalists is mandatory to successfully accomplish the pursued drop or catapult capsule experiment. For this purpose there will be a lot of expertise and help given by ZARM FAB mbH in strong cooperation to-gether with the experimentalists. However, in comparison to standard laboratory setups the drop or catapult capsule setup seems to be completely different at first view. While defining a

  19. [Optimize dropping process of Ginkgo biloba dropping pills by using design space approach].

    Science.gov (United States)

    Shen, Ji-Chen; Wang, Qing-Qing; Chen, An; Pan, Fang-Lai; Gong, Xing-Chu; Qu, Hai-Bin

    2017-07-01

    In this paper, a design space approach was applied to optimize the dropping process of Ginkgo biloba dropping pills. Firstly, potential critical process parameters and potential process critical quality attributes were determined through literature research and pre-experiments. Secondly, experiments were carried out according to Box-Behnken design. Then the critical process parameters and critical quality attributes were determined based on the experimental results. Thirdly, second-order polynomial models were used to describe the quantitative relationships between critical process parameters and critical quality attributes. Finally, a probability-based design space was calculated and verified. The verification results showed that efficient production of Ginkgo biloba dropping pills can be guaranteed by operating within the design space parameters. The recommended operation ranges for the critical dropping process parameters of Ginkgo biloba dropping pills were as follows: dropping distance of 5.5-6.7 cm, and dropping speed of 59-60 drops per minute, providing a reference for industrial production of Ginkgo biloba dropping pills. Copyright© by the Chinese Pharmaceutical Association.

  20. Stress Drops for Potentially Induced Earthquake Sequences

    Science.gov (United States)

    Huang, Y.; Beroza, G. C.; Ellsworth, W. L.

    2015-12-01

    Stress drop, the difference between shear stress acting across a fault before and after an earthquake, is a fundamental parameter of the earthquake source process and the generation of strong ground motions. Higher stress drops usually lead to more high-frequency ground motions. Hough [2014 and 2015] observed low intensities in "Did You Feel It?" data for injection-induced earthquakes, and interpreted them to be a result of low stress drops. It is also possible that the low recorded intensities could be a result of propagation effects. Atkinson et al. [2015] show that the shallow depth of injection-induced earthquakes can lead to a lack of high-frequency ground motion as well. We apply the spectral ratio method of Imanishi and Ellsworth [2006] to analyze stress drops of injection-induced earthquakes, using smaller earthquakes with similar waveforms as empirical Green's functions (eGfs). Both the effects of path and linear site response should be cancelled out through the spectral ratio analysis. We apply this technique to the Guy-Greenbrier earthquake sequence in central Arkansas. The earthquakes migrated along the Guy-Greenbrier Fault while nearby injection wells were operating in 2010-2011. Huang and Beroza [GRL, 2015] improved the magnitude of completeness to about -1 using template matching and found that the earthquakes deviated from Gutenberg-Richter statistics during the operation of nearby injection wells. We identify 49 clusters of highly similar events in the Huang and Beroza [2015] catalog and calculate stress drops using the source model described in Imanishi and Ellsworth [2006]. Our results suggest that stress drops of the Guy-Greenbrier sequence are similar to tectonic earthquakes at Parkfield, California (the attached figure). We will also present stress drop analysis of other suspected induced earthquake sequences using the same method.

  1. Drop impact entrapment of bubble rings

    KAUST Repository

    Thoraval, M.-J.

    2013-04-29

    We use ultra-high-speed video imaging to look at the initial contact of a drop impacting on a liquid layer. We observe experimentally the vortex street and the bubble-ring entrapments predicted numerically, for high impact velocities, by Thoraval et al. (Phys. Rev. Lett., vol. 108, 2012, article 264506). These dynamics mainly occur within 50 -s after the first contact, requiring imaging at 1 million f.p.s. For a water drop impacting on a thin layer of water, the entrapment of isolated bubbles starts through azimuthal instability, which forms at low impact velocities, in the neck connecting the drop and pool. For Reynolds number Re above -12 000, up to 10 partial bubble rings have been observed at the base of the ejecta, starting when the contact is -20% of the drop size. More regular bubble rings are observed for a pool of ethanol or methanol. The video imaging shows rotation around some of these air cylinders, which can temporarily delay their breakup into micro-bubbles. The different refractive index in the pool liquid reveals the destabilization of the vortices and the formation of streamwise vortices and intricate vortex tangles. Fine-scale axisymmetry is thereby destroyed. We show also that the shape of the drop has a strong influence on these dynamics. 2013 Cambridge University Press.

  2. Drop Testing Representative Multi-Canister Overpacks

    Energy Technology Data Exchange (ETDEWEB)

    Snow, Spencer D. [Idaho National Lab. (INL), Idaho Falls, ID (United States); Morton, Dana K. [Idaho National Lab. (INL), Idaho Falls, ID (United States)

    2015-06-01

    The objective of the work reported herein was to determine the ability of the Multi- Canister Overpack (MCO) canister design to maintain its containment boundary after an accidental drop event. Two test MCO canisters were assembled at Hanford, prepared for testing at the Idaho National Engineering and Environmental Laboratory (INEEL), drop tested at Sandia National Laboratories, and evaluated back at the INEEL. In addition to the actual testing efforts, finite element plastic analysis techniques were used to make both pre-test and post-test predictions of the test MCOs structural deformations. The completed effort has demonstrated that the canister design is capable of maintaining a 50 psig pressure boundary after drop testing. Based on helium leak testing methods, one test MCO was determined to have a leakage rate not greater than 1x10-5 std cc/sec (prior internal helium presence prevented a more rigorous test) and the remaining test MCO had a measured leakage rate less than 1x10-7 std cc/sec (i.e., a leaktight containment) after the drop test. The effort has also demonstrated the capability of finite element methods using plastic analysis techniques to accurately predict the structural deformations of canisters subjected to an accidental drop event.

  3. Spread of pathogens through rain drop impact

    Science.gov (United States)

    Kim, Seungho; Gruszewski, Hope; Gidley, Todd; Schmale, David G., III; Jung, Sunghwan

    2017-11-01

    Rain drop impact can disperse micron-sized pathogenic particles over long distances. In this study, we aim to elucidate mechanisms for disease dispersal when a rain drop impacts a particle-laden solid surface. Three different dispersal types were observed depending on whether the dispersed glass particles were dry or wet. For a dry particle dispersal, the movement of contact line made the particles initially jump off the surface with relatively high velocity. Then, air vortex was formed due to the air current entrained along with the falling drop, and advected the particles with relatively low velocity. For a wet particle dispersal, the contact line of a spreading liquid became unstable due to the presence of the particles on the substrate. This caused splashing at the contact line and ejected liquid droplets carrying the particles. Finally, we released a drop onto wheat plants infected with the rust fungus, Puccinia triticina, and found that nearly all of the satellite droplets from a single drop contained at least one rust spore. Also, we visualized such novel dispersal dynamics with a high-speed camera and characterized their features by scaling models. This research was partially supported by National Science Foundation Grant CBET-1604424.

  4. Drop impact on spherical soft surfaces

    Science.gov (United States)

    Chen, Simeng; Bertola, Volfango

    2017-08-01

    The impact of water drops on spherical soft surfaces is investigated experimentally through high-speed imaging. The effect of a convex compliant surface on the dynamics of impacting drops is relevant to various applications, such as 3D ink-jet printing, where drops of fresh material impact on partially cured soft substrates with arbitrary shape. Several quantities which characterize the morphology of impacting drops are measured through image-processing, including the maximum and minimum spreading angles, length of the wetted curve, and dynamic contact angle. In particular, the dynamic contact angle is measured using a novel digital image-processing scheme based on a goniometric mask, which does not require edge fitting. It is shown that the surface with a higher curvature enhances the retraction of the spreading drop; this effect may be due to the difference of energy dissipation induced by the curvature of the surface. In addition, the impact parameters (elastic modulus, diameter ratio, and Weber number) are observed to significantly affect the dynamic contact angle during impact. A quantitative estimation of the deformation energy shows that it is significantly smaller than viscous dissipation.

  5. Spreading of liquid drop on superhydrophilic micropillar array

    Science.gov (United States)

    Kim, Seong Jin; Moon, Myoung-Woon; Lee, Kwang-Ryeol; Kim, Ho-Young

    2012-11-01

    When a drop is deposited on a superhydrophilic micropillar array, the upper part of the drop (referred to as the bulk) collapses while the bottom part penetrates into the gaps of the array, forming a fringe film. Here we quantify the dynamics of this process using a combination of experiment and theory. In the early stages when the fringe extension is negligible compared to the bulk radius, both the spreading of the bulk and the entire drop footprint follow the same power law (t 1 / 4), t being time. The bulk shrinks toward the end of the spreading process due to the drainage of liquid into the fringe film. The film spreads like t 1 / 2 until the end of the process. A remarkable finding is that the entire footprint grows like t 1 / 4 despite the diffusive growth of the fringe film, implying that the shrinkage of the bulk compensates for the outward spreading of the film. We rationalize some of these results with scaling analyses based on the balance of capillary forces that drive the flow and viscous shear forces.

  6. Seismic II over I Drop Test Program results and interpretation

    International Nuclear Information System (INIS)

    Thomas, B.

    1993-03-01

    The consequences of non-seismically qualified (Category 2) objects falling and striking essential seismically qualified (Category 1) objects has always been a significant, yet analytically difficult problem, particularly in evaluating the potential damage to equipment that may result from earthquakes. Analytical solutions for impact problems are conservative and available for mostly simple configurations. In a nuclear facility, the open-quotes sourcesclose quotes and open-quotes targetsclose quotes requiring evaluation are frequently irregular in shape and configuration, making calculations and computer modeling difficult. Few industry or regulatory rules are available on this topic even though it is a source of considerable construction upgrade costs. A drop test program was recently conducted to develop a more accurate understanding of the consequences of seismic interactions. The resulting data can be used as a means to improve the judgment of seismic qualification engineers performing interaction evaluations and to develop realistic design criteria for seismic interactions. Impact tests on various combinations of sources and targets commonly found in one Savannah River Site (SRS) nuclear facility were performed by dropping the sources from various heights onto the targets. This report summarizes results of the Drop Test Program. Force and acceleration time history data are presented as well as general observations on the overall ruggedness of various targets when subjected to impacts from different types of sources

  7. Drop weld thermal injuries to the middle ear.

    LENUS (Irish Health Repository)

    Keogh, I J

    2009-01-01

    Drop weld injuries to the tympanic membrane and middle ear caused by hot sparks or molten slag are a rare but significant injury. Steel workers and welders who are regularly exposed to flying sparks and molten metal slag are predisposed. This type of transtympanic thermal injury occurs when the slag literally drops into the external auditory canal and burns through the tympanic membrane. A spectrum of severity of injury occurs which includes chronic tympanic membrane perforation, chronic otorrhoea, facial nerve injury and deafness. Chronic tympanic membrane perforation is the most common sequelae and is perhaps one of the most challenging of all perforations to repair The combination of direct thermal injury and foreign body reaction results in continuing or recurrent suppuration. The foreign body reaction is due to the embedding of metal slag in the promontorial mucosa. We present a case of drop weld injury to the left tympanic membrane, resulting in chronic middle ear inflammation, otorrhoea and tympanic perforation. CAT scan clearly demonstrated a metallic promontorial foreign body with localised bone erosion. We emphasise the importance of removing these foreign bodies and recommend a cartilage reinforced underlay tympanoplasty technique to repair these perforations. Transtympanic thermal trauma is a preventable occupational injury, which is best, avoided by earplugs and increased awareness.

  8. Pesticide extraction from table grapes and plums using ionic liquid based dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Ravelo-Pérez, Lidia M; Hernández-Borges, Javier; Herrera-Herrera, Antonio V; Rodríguez-Delgado, Miguel Angel

    2009-12-01

    Room temperature ionic liquids (RTILs) have been used as extraction solvents in dispersive liquid-liquid microextraction (DLLME) for the determination of eight multi-class pesticides (i.e. thiophanate-methyl, carbofuran, carbaryl, tebuconazole, iprodione, oxyfluorfen, hexythiazox, and fenazaquin) in table grapes and plums. The developed method involves the combination of DLLME and high-performance liquid chromatography with diode array detection. Samples were first homogenized and extracted with acetonitrile. After evaporation and reconstitution of the extract in water containing sodium chloride, a quick DLLME procedure that used the ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate ([C(6)MIM][PF(6)]) and methanol was developed. The RTIL dissolved in a very small volume of acetonitrile was directed injected in the chromatographic system. The comparison between the calibration curves obtained from standards and from spiked sample extracts (matrix-matched calibration) showed the existence of a strong matrix effect for most of the analyzed pesticides. A recovery study was also developed with five consecutive extractions of the two types of fruits spiked at three concentration levels. Mean recovery values were in the range of 72-100% for table grapes and 66-105% for plum samples (except for thiophanate-methyl and carbofuran, which were 64-75% and 58-66%, respectively). Limits of detection (LODs) were in the range 0.651-5.44 microg/kg for table grapes and 0.902-6.33 microg/kg for plums, representing LODs below the maximum residue limits (MRLs) established by the European Union in these fruits. The potential of the method was demonstrated by analyzing 12 commercial fruit samples (six of each type).

  9. Trace determination of volatile polycyclic aromatic hydrocarbons in natural waters by magnetic ionic liquid-based stir bar dispersive liquid microextraction.

    Science.gov (United States)

    Benedé, Juan L; Anderson, Jared L; Chisvert, Alberto

    2018-01-01

    In this work, a novel hybrid approach called stir bar dispersive liquid microextraction (SBDLME) that combines the advantages of stir bar sorptive extraction (SBSE) and dispersive liquid-liquid microextraction (DLLME) has been employed for the accurate and sensitive determination of ten polycyclic aromatic hydrocarbons (PAHs) in natural water samples. The extraction is carried out using a neodymium stir bar magnetically coated with a magnetic ionic liquid (MIL) as extraction device, in such a way that the MIL is dispersed into the solution at high stirring rates. Once the stirring is ceased, the MIL is magnetically retrieved onto the stir bar, and subsequently subjected to thermal desorption (TD) coupled to a gas chromatography-mass spectrometry (GC-MS) system. The main parameters involved in TD, as well as in the extraction step affecting the extraction efficiency (i.e., MIL amount, extraction time and ionic strength) were evaluated. Under the optimized conditions, the method was successfully validated showing good linearity, limits of detection and quantification in the low ng L -1 level, good intra- and inter-day repeatability (RSD < 13%) and good enrichment factors (18 - 717). This sensitive analytical method was applied to the determination of trace amounts of PAHs in three natural water samples (river, tap and rainwater) with satisfactory relative recovery values (84-115%), highlighting that the matrices under consideration do not affect the extraction process. Copyright © 2017 Elsevier B.V. All rights reserved.

  10. Rapid determination of some psychotropic drugs in complex matrices by tandem dispersive liquid-liquid microextraction followed by high performance liquid chromatography.

    Science.gov (United States)

    Asghari, Alireza; Fahimi, Ebrahim; Bazregar, Mohammad; Rajabi, Maryam; Boutorabi, Leila

    2017-05-01

    Simple and rapid determinations of some psychotropic drugs in some pharmaceutical wastewater and human plasma samples were successfully accomplished via the tandem dispersive liquid-liquid microextraction combined with high performance liquid chromatography-ultraviolet detection (TDLLME-HPLC-UV). TDLLME of the three psychotropic drugs clozapine, chlorpromazine, and thioridazine was easily performed through two consecutive dispersive liquid-liquid microextractions. By performing this convenient method, proper sample preconcentrations and clean-ups were achieved in just about 7min. In order to achieve the best extraction efficiency, the effective parameters involved were optimized. The optimal experimental conditions consisted of 100μL of CCl 4 (as the extraction organic solvent), and the pH values of 13 and 2 for the donor and acceptor phases, respectively. Under these optimum experimental conditions, the proposed TDLLME-HPLC-UV technique provided a good linearity in the range of 5-3000ngmL -1 for the three psychotropic drugs with the correlation of determinations (R 2 s) higher than 0.996. The limits of quantification (LOQs) and limits of detection (LODs) obtained were 5.0ngmL -1 and 1.0-1.5ngmL -1 , respectively. Also the proper enrichment factors (EFs) of 96, 99, and 88 for clozapine, chlorpromazine, and thioridazine, respectively, and good extraction repeatabilities (relative standard deviations below 9.3%, n=5) were obtained. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Comparison of two novel in-syringe dispersive liquid-liquid microextraction techniques for the determination of iodide in water samples using spectrophotometry.

    Science.gov (United States)

    Kaykhaii, Massoud; Sargazi, Mona

    2014-01-01

    Two new, rapid methodologies have been developed and applied successfully for the determination of trace levels of iodide in real water samples. Both techniques are based on a combination of in-syringe dispersive liquid-liquid microextraction (IS-DLLME) and micro-volume UV-Vis spectrophotometry. In the first technique, iodide is oxidized with nitrous acid to the colorless anion of ICl2(-) at high concentration of hydrochloric acid. Rhodamine B is added and by means of one step IS-DLLME, the ion-pair formed was extracted into toluene and measured spectrophotometrically. Acetone is used as dispersive solvent. The second method is based on the IS-DLLME microextraction of iodide as iodide/1, 10-phenanthroline-iron((II)) chelate cation ion-pair (colored) into nitrobenzene. Methanol was selected as dispersive solvent. Optimal conditions for iodide extraction were determined for both approaches. Methods are compared in terms of analytical parameters such as precision, accuracy, speed and limit of detection. Both methods were successfully applied to determining iodide in tap and river water samples. Copyright © 2013 Elsevier B.V. All rights reserved.

  12. Determination of four sulfonylurea herbicides in tea by matrix solid-phase dispersion cleanup followed by dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Liang, Pei; Wang, Jinjin; Liu, Guojiao; Guan, Jinyan

    2014-09-01

    Matrix solid-phase dispersion combined with dispersive liquid-liquid microextraction has been developed as a new sample pretreatment method for the determination of four sulfonylurea herbicides (chlorsulfuron, bensulfuron-methyl, chlorimuron-ethyl, and pyrazosulfuron) in tea by high-performance liquid chromatography with diode array detection. The extraction and cleanup by matrix solid-phase dispersion was carried out by using CN-silica as dispersant and carbon nanotubes as cleanup sorbent eluted with acidified dichloromethane. The eluent of matrix solid-phase dispersion was evaporated and redissolved in 0.5 mL methanol, and used as the dispersive solvent of the following dispersive liquid-liquid microextraction procedure for further purification and enrichment of the target analytes before high-performance liquid chromatography analysis. Under the optimum conditions, the method yielded a linear calibration curve in the concentration range from 5.0 to 10 000 ng/g for target analytes with a correlation coefficients (r(2)) ranging from 0.9959 to 0.9998. The limits of detection for the analytes were in the range of 1.31-2.81 ng/g. Recoveries of the four sulfonylurea herbicides at two fortification levels were between 72.8 and 110.6% with relative standard deviations lower than 6.95%. The method was successfully applied to the analysis of four sulfonylurea herbicides in several tea samples. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. A dispersive liquid--liquid microextraction methodology for copper (II) in environmental samples prior to determination using microsample injection flame atomic absorption spectrometry.

    Science.gov (United States)

    Alothman, Zeid A; Habila, Mohamed; Yilmaz, Erkan; Soylak, Mustafa

    2013-01-01

    A simple, environmentally friendly, and efficient dispersive liquid-liquid microextraction method combined with microsample injection flame atomic absorption spectrometry was developed for the separation and preconcentration of Cu(II). 2-(5-Bromo-2-pyridylazo)-5-(diethylamino)phenol (5-Br-PADAP) was used to form a hydrophobic complex of Cu(II) ions in the aqueous phase before extraction. To extract the Cu(II)-5-Br-PADAP complex from the aqueous phase to the organic phase, 2.0 mL of acetone as a disperser solvent and 200 microL of chloroform as an extraction solvent were used. The influences of important analytical parameters, such as the pH, types and volumes of the extraction and disperser solvents, amount of chelating agent, sample volume, and matrix effects, on the microextraction procedure were evaluated and optimized. Using the optimal conditions, the LOD, LOQ, preconcentration factor, and RSD were determined to be 1.4 microg/L, 4.7 microg/L, 120, and 6.5%, respectively. The accuracy of the proposed method was investigated using standard addition/recovery tests. The analysis of certified reference materials produced satisfactory analytical results. The developed method was applied for the determination of Cu in real samples.

  14. Simultaneous Pre-Concentration of Cadmium and Lead in Environmental Water Samples with Dispersive Liquid-Liquid Microextraction and Determination by Inductively Coupled Plasma-Atomic Emission Spectrometry

    Directory of Open Access Journals (Sweden)

    M. Salahinejad

    2013-06-01

    Full Text Available The dispersive liquid–liquid microextraction (DLLME method for determination of Pb+2 and Cd+2 ions in the environmental water samples was combined with inductively coupled plasma-atomic emission spectrometry (ICP-AES. Ammonium pyrrolidine dithiocarbamate (APDC, chloroform and ethanol were used as chelating agent, extraction solvent and disperser solvent, respectively. Some effective parameters on the microextraction and the complex formation were selected and optimized. These parameters included extraction and disperser solvent type as well as their volume, extraction time, salt effect, pH, sample volume and amount of the chelating agent.   Under the optimum conditions, the enrichment factor of 75 and 105 for Cd+2 and Pb+2 ions respectively was obtained from only 5.00mL of water sample. The detection limit (S/N=3 was 12 and 0.8ngmL−1 for Pb and Cd respectively. The relative standard deviation (RSDs for five replicate measurements of 0.50 mgL−1 of lead and cadmium was 6.5 and 4.4 % respectively. Mineral, tap, river, sea, dam and spiked water samples were analyzed for Cd and Pb amount.

  15. Ultrasonic characterization of single drops of liquids

    Energy Technology Data Exchange (ETDEWEB)

    Sinha, Dipen N. (Los Alamos, NM)

    1998-01-01

    Ultrasonic characterization of single drops of liquids. The present invention includes the use of two closely spaced transducers, or one transducer and a closely spaced reflector plate, to form an interferometer suitable for ultrasonic characterization of droplet-size and smaller samples without the need for a container. The droplet is held between the interferometer elements, whose distance apart may be adjusted, by surface tension. The surfaces of the interferometer elements may be readily cleansed by a stream of solvent followed by purified air when it is desired to change samples. A single drop of liquid is sufficient for high-quality measurement. Examples of samples which may be investigated using the apparatus and method of the present invention include biological specimens (tear drops; blood and other body fluid samples; samples from tumors, tissues, and organs; secretions from tissues and organs; snake and bee venom, etc.) for diagnostic evaluation, samples in forensic investigations, and detection of drugs in small quantities.

  16. Superheated drop as a neutron spectrometer

    Science.gov (United States)

    Das, Mala; Chatterjee, B. K.; Roy, B.; Roy, S. C.

    2000-09-01

    Superheated drops are known to vaporise when exposed to energetic nuclear radiation since the discovery of bubble chamber. The application of superheated drops in neutron research especially in neutron dosimetry is a subject of intense research for quite sometime. As the degree of superheat increases in a given liquid, less and less energetic neutrons are required to cause nucleation. This property of superheated liquid makes it possible to use it as a neutron spectrometer. Neutron detection efficiency of superheated drops made of R12 exposed to Am-Be neutron source has been measured over a wide range of temperature -17-60°C and the results have been utilised to construct the energy spectrum of the neutron source. This paper demonstrates that a suitable neutron spectrometer may be constructed by using a single liquid and varying the temperature of the liquid suitably at a closer grid.

  17. Superheated drop as a neutron spectrometer

    Energy Technology Data Exchange (ETDEWEB)

    Das, Mala; Chatterjee, B.K.; Roy, B. E-mail: biva@bosemain.boseinst.ernet.in; Roy, S.C

    2000-09-21

    Superheated drops are known to vaporise when exposed to energetic nuclear radiation since the discovery of bubble chamber. The application of superheated drops in neutron research especially in neutron dosimetry is a subject of intense research for quite sometime. As the degree of superheat increases in a given liquid, less and less energetic neutrons are required to cause nucleation. This property of superheated liquid makes it possible to use it as a neutron spectrometer. Neutron detection efficiency of superheated drops made of R12 exposed to Am-Be neutron source has been measured over a wide range of temperature -17-60 deg. C and the results have been utilised to construct the energy spectrum of the neutron source. This paper demonstrates that a suitable neutron spectrometer may be constructed by using a single liquid and varying the temperature of the liquid suitably at a closer grid.

  18. Tunable Transport of Drops on a Vibrating Fiber

    Science.gov (United States)

    Bick, Alison; Sauret, Alban; Boulogne, Francois; Stone, Howard

    2014-11-01

    Transport of liquid drops on a fibrous medium is common in engineering systems such as fog harvesting and textile cleaning. The control of the drop movement on fibrous media can make these engineering systems more efficient. We investigated how to move drops along a single inclined fiber by controlling fiber vibration. Drop motion: static, sliding or falling, depends on the fiber inclination angle, drop volume, and the distance of the drop from the vibrating source. Specifically, by vibrating the fiber the transition between the three drop motion states can be controlled. By defining the response of drop movement to vibration frequency, we can model the drop movement transition. This knowledge is directly useful for controlling drop movement on the fiber. In particular, we experimentally demonstrated that vibration frequency can be used to transport a drop along a fiber.

  19. Alternative drop-set – occlusion eccentric-ballistic method

    OpenAIRE

    Mirzayev, Javid Azerovich

    2018-01-01

    Annotation. This article talks about a method that combines the following elements: 1) the pace of execution; 2) the KAATSU method; 3) drop-set. The rate of movement is one of the most important training variables. After all, many motor activities, whether in sports of higher achievements or in physical culture, take place in a shorter time interval than the muscles on the way to obtaining maximum production of force. The pace of implementation is an very important factor, related to the deve...

  20. Shuttlecock Velocity of a Badminton Drop Shot

    Directory of Open Access Journals (Sweden)

    Ampharin Ongvises

    2013-12-01

    Full Text Available In a badminton ‘drop shot’, the shuttlecock is struck by a non-rotating racquet at low speed. In this investigation, a shuttlecock was hit by a badminton racquet in a linear collision, simulating a drop shot. The collision was recorded with high-speed video and the velocities of the racquet and shuttlecock determined. The relationship between the impact velocity of the racquet and the velocity of the shuttlecock as it leaves the badminton racquet after collision was found to be proportional over the range tested.

  1. Speciation analysis of aqueous nanoparticulate diclofenac complexes by solid-phase microextraction

    NARCIS (Netherlands)

    Zielinska, K.; Leeuwen, van H.P.; Thibault, S.; Town, R.M.

    2012-01-01

    The dynamic sorption of an organic compound by nanoparticles (NPs) is analyzed by solid-phase microextraction (SPME) for the example case of the pharmaceutical diclofenac in dispersions of impermeable (silica, SiO(2)) and permeable (bovine serum albumin, BSA) NPs. It is shown that only the

  2. Micro-Lid For Sealing Sample Reservoirs of micro-Extraction Systems

    Data.gov (United States)

    National Aeronautics and Space Administration — We propose to develop a proof-of-concept micro-Lid (µLid) to tightly seal a micro-sampler or micro-extraction system. Fabrication of µLid would be conducted in the...

  3. Solid phase microextraction speciation analysis of triclosan in aqueous mediacontaining sorbing nanoparticles

    NARCIS (Netherlands)

    Zielinska, K.

    2014-01-01

    Solid phase microextraction (SPME) is applied in the speciation analysis of the hydrophobic compound triclosan in an aqueous medium containing sorbing SiO2 nanoparticles (NPs). It is found that these NPs, as well as their complexes with triclosan, partition between the bulk medium and the solid

  4. Critical micelle concentration values for different surfactants measured with solid-phase microextraction fibers

    NARCIS (Netherlands)

    Haftka, Joris J H; Scherpenisse, Peter; Oetter, G??nter; Hodges, Geoff; Eadsforth, Charles V.; Kotthoff, Matthias; Hermens, Joop L M

    The amphiphilic nature of surfactants drives the formation of micelles at the critical micelle concentration (CMC). Solid-phase microextraction (SPME) fibres were used in the present study to measure CMC values of twelve nonionic, anionic, cationic and zwitterionic surfactants. The SPME derived CMC

  5. Experimental validation of plugging during drop formation in a T-junction.

    Science.gov (United States)

    Abate, Adam R; Mary, Pascaline; van Steijn, Volkert; Weitz, David A

    2012-04-21

    At low capillary number, drop formation in a T-junction is dominated by interfacial effects: as the dispersed fluid flows into the drop maker nozzle, it blocks the path of the continuous fluid; this leads to a pressure rise in the continuous fluid that, in turn, squeezes on the dispersed fluid, inducing pinch-off of a drop. While the resulting drop volume predicted by this "squeezing" mechanism has been validated for a range of systems, as of yet, the pressure rise responsible for the actual pinch-off has not been observed experimentally. This is due to the challenge of measuring the pressures in a T-junction with the requisite speed, accuracy, and localization. Here, we present an empirical study of the pressures in a T-junction during drop formation. Using Laplace sensors, pressure probes we have developed, we confirm the central ideas of the squeezing mechanism; however, we also uncover other findings, including that the pressure of the dispersed fluid is not constant but rather oscillates in anti-phase with that of the continuous fluid. In addition, even at the highest capillary number for which monodisperse drops can be formed, pressure oscillations persist, indicating that drop formation in confined geometries does not transition to an entirely shear-driven mechanism, but to a mechanism combining squeezing and shearing.

  6. Curative effect of Sodium hyaluronate and bFGF eye drops after corneal rust foreign body removal operation

    Directory of Open Access Journals (Sweden)

    Jin-Xia Li1

    2013-10-01

    Full Text Available AIM: To observe the combined effect of Sodium hyaluronate eye drops and recombinant bovine basic fibroblast growth factor(bFGFeye drops on cornea epithelial repair after corneal rust foreign body extraction. METHODS: Alinety-eight cases(98 eyesof corneal rust foreign body patients were randomly distributed to combined treatment group(49 cases, 49 eyesand control group(49 cases, 49 eyes. Hyaluronate eye drops, recombinant bFGF eye drops and levofloxacin hydrochloride were applied in combined treatment group after corneal foreign body extraction. Recombinant bFGF eye drops and levofloxacin hydrochloride were applied in control group. Corneal fluorescein stain, cornea epithelial repair and local symptoms were examined thrice weekly for 2 weeks. RESULTS: General effective rate of treatment in combined group reach 96%, significantly higher than that in control group(88%, PCONCLUSION: Combined application of sodium hyaluronate eye drops and recombinant bFGF eye drops can prominently improve cornea epithelial repair after corneal lesion with proven effectiveness and safety.

  7. An evaporation model of multicomponent solution drops

    Science.gov (United States)

    Sartori, Silvana; Liñán, Amable; Lasheras, Juan C.

    2010-11-01

    Solutions of polymers are widely used in the pharmaceutical industry as tablets coatings. These allow controlling the rate at which the drug is delivered, taste or appearance. The coating is performed by spraying and drying the tablets at moderate temperatures. The wetting of the coating solution on the pill's surface depends on the droplet Webber and Re numbers, angle of impact and on the rheological properties of the droplet. We present a model for the evaporation of multicomponent solutions droplets in a hot air environment with temperatures substantially lower than the boiling temperature of the solvent. As the liquid vaporizes from the surface the fluid in the drop increases in concentration, until reaching its saturation point. After saturation, precipitation occurs uniformly within the drop. As the surface regresses, a compacting front formed by the precipitate at its maximum packing density advances into the drop, while the solute continues precipitating uniformly. This porous shell grows fast due to the double effect of surface regression and precipitation. The evaporation rate is determined by the rates at which heat is transported to the droplet surface and at which liquid vapor diffuses away from it. When the drop is fully compacted, the evaporation is drastically reduced.

  8. Spontaneous evaporation of the acetone drop

    Science.gov (United States)

    Dunin, S. Z.; Nagornov, O. V.

    2017-12-01

    The exact solution of the problem on evaporation of the acetone sessile drop at solid substrate is derived. The solution allows us to analyze the temperature field behavior at various thermodynamic parameters. The Marangoni forces are calculated in explicit form. The solution can be used to check numerical approaches for similar problems.

  9. Check valves with drop-shaped disk

    Energy Technology Data Exchange (ETDEWEB)

    1943-03-19

    This report discusses improvements possible with drop check valves. Up to the time of the report, the most important improvements had been: (1) lightening of the drop by hollowing it out, (2) reducing lift to reduce impact, (3) increasing clearance in the guide to minimize the danger of it getting stuck, (4) drilling of a safety hole which would indicate excessive wear of the housing by a leak. Other possibilities for the above improvements had produced the following conclusions: (1) a further lightening of the drop was found possible by milling out the halves with a milling cutter, by welding them together and thus eliminating the threaded portion, or by having the drop open on the bottom; (2) further reduction in lift was not found possible in most sizes, but for reduction of the impact effect by a cushion of oil or paste, the seating surface was widened as much as possible; (3) sticking of certain check valves caused by ferrous sulfide deposits could be solved by use of a certain bushing in the housing; (4) some plants favored and some disfavored the safety hole, but in general, plants were to service check valves and change them at such regular intervals as experience dictated; (5) the seat plate was no longer solid steel, but a welded piece.

  10. Goose droppings as food for reindeer

    NARCIS (Netherlands)

    van der Wal, R; Loonen, MJJE

    Feeding conditions for Svalbard reindeer, Rangifer tarandus platyrhynchus, on Spitsbergen are generally poor, owing to low availability of forage. We report on coprophagy: the use of goose faeces as an alternative food source for reindeer. Fresh droppings from Barnacle Geese, Branta leucopsis,

  11. Modeling merging behavior at lane drops.

    Science.gov (United States)

    2015-02-01

    In work-zone configurations where lane drops are present, merging of traffic at the taper presents an operational concern. In : addition, as flow through the work zone is reduced, the relative traffic safety of the work zone is also reduced. Improvin...

  12. 49 CFR 178.603 - Drop test.

    Science.gov (United States)

    2010-10-01

    ... of natural wood, Plywood boxes, Reconstituted wood boxes, Fiberboard boxes, Plastic boxes, Steel or... drums, Plastic drums and Jerricans, Composite packagings which are in the shape of a drum Six—(three for... Administrator. (c) Special preparation of test samples for the drop test. (1) Testing of plastic drums, plastic...

  13. 49 CFR 178.965 - Drop test.

    Science.gov (United States)

    2010-10-01

    ... Large Packaging design types and performed periodically as specified in § 178.955(e) of this subpart. (b... § 178.960(d). (d) Test method. (1) Samples of all Large Packaging design types must be dropped onto a... be restored to the upright position for observation. (2) Large Packaging design types with a capacity...

  14. The initial regime of drop coalescence

    Science.gov (United States)

    Anthony, Christopher; Harris, Michael; Basaran, Osman

    2017-11-01

    Drop coalescence plays a key role in both industry and nature. Consequently, study of the phenomenon has been the focus of numerous experimental, computational and theoretical works to date. In coalescence, two drops come into contact and a liquid bridge forms between them. As time advances, this bridge grows from microscopic to macroscopic scales. Despite the large volume of work dedicated to this problem, currently experiment, theory, and computation are not in perfect agreement with respect to the earliest times following the initial contact of the drops. Experiments report an initial regime where the radius of the connecting bridge grows linearly in time before a transition to either a Stokes regime or an inertial regime where either viscous or inertial forces balance capillary force. In the initial linear regime, referred to as the inertially-limited viscous regime, all three forces are thought to be important. This is in contrast to theory which predicts that all coalescence events begin in the Stokes regime. We use high accuracy numerical simulation to show that the existing discrepancy in the literature can be resolved by paying careful attention to the initial conditions that set the shape and size of the bridge connecting the two drops.

  15. The stability of cylindrical pendant drops

    CERN Document Server

    McCuan, John

    2018-01-01

    The author considers the stability of certain liquid drops in a gravity field satisfying a mixed boundary condition. He also considers as special cases portions of cylinders that model either the zero gravity case or soap films with the same kind of boundary behavior.

  16. Reactor Flow and Pressure Drop Study

    Energy Technology Data Exchange (ETDEWEB)

    Keyes, R. E.

    1969-07-15

    A study was made to determine the flow rates and pressure drops for all primary system flow paths through the FTR. The main data and results are in tables, diagrams and curves. The results are intended to provide a common basis for evaluation of parametric changes in the system.

  17. Biomechanical analysis of drop and countermovement jumps

    NARCIS (Netherlands)

    Bobbert, M. F.; Mackay, M.T.; Schinkelshoek, D.; Huijing, P. A.; van Ingen Schenau, G. J.

    For 13 subjects the performance of drop jumps from a height of 40 cm (DJ) and of countermovement jumps (CMJ) was analysed and compared. From force plate and cine data biomechanical variables including forces, moments, power output and amount of work done were calculated for hip, knee and ankle

  18. Scaling the drop size in coflow experiments

    International Nuclear Information System (INIS)

    Castro-Hernandez, E; Gordillo, J M; Gundabala, V; Fernandez-Nieves, A

    2009-01-01

    We perform extensive experiments with coflowing liquids in microfluidic devices and provide a closed expression for the drop size as a function of measurable parameters in the jetting regime that accounts for the experimental observations; this expression works irrespective of how the jets are produced, providing a powerful design tool for this type of experiments.

  19. Scaling the drop size in coflow experiments

    Energy Technology Data Exchange (ETDEWEB)

    Castro-Hernandez, E; Gordillo, J M [Area de Mecanica de Fluidos, Universidad de Sevilla, Avenida de los Descubrimientos s/n, 41092 Sevilla (Spain); Gundabala, V; Fernandez-Nieves, A [School of Physics, Georgia Institute of Technology, Atlanta, GA 30332 (United States)], E-mail: jgordill@us.es

    2009-07-15

    We perform extensive experiments with coflowing liquids in microfluidic devices and provide a closed expression for the drop size as a function of measurable parameters in the jetting regime that accounts for the experimental observations; this expression works irrespective of how the jets are produced, providing a powerful design tool for this type of experiments.

  20. Electrostatic potential wells for on-demand drop manipulation in microchannels.

    Science.gov (United States)

    de Ruiter, Riëlle; Pit, Arjen M; de Oliveira, Vitor Martins; Duits, Michèl H G; van den Ende, Dirk; Mugele, Frieder

    2014-03-07

    Precise control and manipulation of individual drops are crucial in many lab-on-a-chip applications. We present a novel hybrid concept for channel-based discrete microfluidics with integrated electrowetting functionality by incorporating co-planar electrodes (separated by a narrow gap) in one of the microchannel walls. By combining the high throughput of channel-based microfluidics with the individual drop control achieved using electrical actuation, we acquire the strengths of both worlds. The tunable strength of the electrostatic forces enables a wide range of drop manipulations, such as on-demand trapping and release, guiding, and sorting of drops in the microchannel. In each of these scenarios, the retaining electrostatic force competes with the hydrodynamic drag force. The conditions for trapping can be predicted using a simple model that balances these forces.

  1. Ordered mesoporous carbon film as an effective solid-phase microextraction coating for determination of benzene series from aqueous media

    Energy Technology Data Exchange (ETDEWEB)

    Jiang, Hui [Jiangsu Key Laboratory of Chemical Pollution Control and Resources Reuse, School of Environmental Science and Engineering, Nanjing University of Science and Technology, Nanjing 210094 (China); School of Geography Science, Nantong University, Nantong 226001 (China); Li, Jiansheng, E-mail: lijsh@mail.njust.edu.cn [Jiangsu Key Laboratory of Chemical Pollution Control and Resources Reuse, School of Environmental Science and Engineering, Nanjing University of Science and Technology, Nanjing 210094 (China); Jiang, Mingyue; Lu, Rui; Shen, Jinyou; Sun, Xiuyun; Han, Weiqing [Jiangsu Key Laboratory of Chemical Pollution Control and Resources Reuse, School of Environmental Science and Engineering, Nanjing University of Science and Technology, Nanjing 210094 (China); Wang, Lianjun, E-mail: wanglj@mail.njust.edu.cn [Jiangsu Key Laboratory of Chemical Pollution Control and Resources Reuse, School of Environmental Science and Engineering, Nanjing University of Science and Technology, Nanjing 210094 (China)

    2015-08-12

    The present work reports preparation of ordered mesoporous carbon (OMC) film supported on a graphite fiber as a new type of solid-phase microextraction (SPME) fiber for determination of benzene series from aqueous media. The strategy for the supported OMC film preparation was combined dip-coating technology with solvent evaporation-induced self-assembly (EISA) approach. A graphite fiber was immersed in an ethanol solution containing phenolic resin and Pluronic triblock copolymer. Upon solvent evaporation and subsequent pyrolysis under 700 °C, the phenolic resin and the surfactant self-assembled on the surface of the graphite fiber to form smooth OMC film. X-ray diffraction (XRD), transmission electron microscopy (TEM) and nitrogen isothermal adsorption results indicate that the resultant OMC film possesses well-ordered two dimensional hexagonal mesostructure with pore diameters of 4.5 nm and BET surfaces of 630 m{sup 2}/g. Scanning electron microscopy (SEM) studies show the supported OMC film with thickness at 8.5 μm is continuous and defect-free. The SPME efficiency of the OMC fiber was evaluated by analysis of five benzene series (benzene, toluene, ethylbenzene, p-xylene and m-xylene) from water samples by gas chromatography-flame ionization detection (GC-FID). The analysis results indicate that the prepared OMC fiber has wide linear ranges (0.5–500 μg/L), low detection limits (0.01–0.05 μg/L) and good repeatabilities (4.0–5.8% for one fiber, 2.9–8.7% for fiber-to-fiber). Compared with commercial counterparts, the OMC fiber exhibits improved extraction efficiency for benzene series and PAHs. - Highlights: • Ordered mesoporous carbon film supported on graphite fiber was first reported as solid-phase microextraction coating. • The strategy for the film preparation was combined dip-coating technology with evaporation-induced self-assembly approach. • The obtained fiber showed enhanced thermal stability and organic solvents resistance. • The

  2. Coalescence collision of liquid drops I: Off-center collisions of equal-size drops

    Directory of Open Access Journals (Sweden)

    Alejandro Acevedo-Malavé

    2011-09-01

    Full Text Available The Smoothed Particle Hydrodynamics method (SPH is used here to model off-center collisions of equal-size liquid drops in a three-dimensional space. In this study the Weber number is calculated for several conditions of the droplets dynamics and the velocity vector fields formed inside the drops during the collision process are shown. For the permanent coalescence the evolution of the kinetic and internal energy is shown and also the approaching to equilibrium of the resulting drop. Depending of the Weber number three possible outcomes for the collision of droplets is obtained: permanent coalescence, flocculation and fragmentation. The fragmentation phenomena are modeled and the formation of small satellite drops can be seen. The ligament that is formed follows the “end pinching” mechanism and it is transformed into a flat structure.

  3. Control of Drop Motion by Mechanical Vibrations

    Science.gov (United States)

    Bestehorn, Michael

    2014-11-01

    Since the first experimental observations of Michael Faraday in 1831 it is known that a vibrating liquid may show an instability of its flat free surface with respect to oscillating regular surface patterns. We study thin liquid films on a horizontal substrate in the long wave approximation. The films are parametrically excited by mechanical horizontal or inclined oscillations. Inertia effects are taken into account and the standard thin film formulation is extended by a second equation for the vertically averaged mass flux. The films can be additionally unstable by Van der Waals forces on a partially wetting substrate, leading to the formation of drops. These drops can be manipulated by the vibrations to move in a desired direction. Linear results based on a damped complex valued Mathieu equation as well as fully nonlinear results using a reduced model will be presented, for more details see.

  4. A pressure drop model for PWR grids

    Energy Technology Data Exchange (ETDEWEB)

    Oh, Dong Seok; In, Wang Ki; Bang, Je Geon; Jung, Youn Ho; Chun, Tae Hyun [Korea Atomic Energy Research Institute, Taejon (Korea, Republic of)

    1998-12-31

    A pressure drop model for the PWR grids with and without mixing device is proposed at single phase based on the fluid mechanistic approach. Total pressure loss is expressed in additive way for form and frictional losses. The general friction factor correlations and form drag coefficients available in the open literatures are used to the model. As the results, the model shows better predictions than the existing ones for the non-mixing grids, and reasonable agreements with the available experimental data for mixing grids. Therefore it is concluded that the proposed model for pressure drop can provide sufficiently good approximation for grid optimization and design calculation in advanced grid development. 7 refs., 3 figs., 3 tabs. (Author)

  5. How drops start sliding over solid surfaces

    Science.gov (United States)

    Gao, Nan; Geyer, Florian; Pilat, Dominik W.; Wooh, Sanghyuk; Vollmer, Doris; Butt, Hans-Jürgen; Berger, Rüdiger

    2018-02-01

    It has been known for more than 200 years that the maximum static friction force between two solid surfaces is usually greater than the kinetic friction force--the force that is required to maintain the relative motion of the surfaces once the static force has been overcome. But the forces that impede the lateral motion of a drop of liquid on a solid surface are not as well characterized, and there is a lack of understanding about liquid-solid friction in general. Here, we report that the lateral adhesion force between a liquid drop and a solid can also be divided into a static and a kinetic regime. This striking analogy with solid-solid friction is a generic phenomenon that holds for liquids of different polarities and surface tensions on smooth, rough and structured surfaces.

  6. Drop evaporation and triple line dynamics

    Science.gov (United States)

    Sobac, Benjamin; Brutin, David; Gavillet, Jerome; Université de Provence Team; Cea Liten Team

    2011-03-01

    Sessile drop evaporation is a phenomenon commonly came across in nature or in industry with cooling, paintings or DNA mapping. However, the evaporation of a drop deposited on a substrate is not completely understood due to the complexity of the problem. Here we investigate, with several nano-coating of the substrate (PTFE, SiOx, SiOc and CF), the influence of the dynamic of the triple line on the evaporation process. The experiment consists in analyzing simultaneously the motion of the triple line, the kinetics of evaporation, the internal thermal motion and the heat and mass transfer. Measurements of temperature, heat-flux and visualizations with visible and infrared cameras are performed. The dynamics of the evaporative heat flux appears clearly different depending of the motion of the triple line

  7. Semisupervised Community Detection by Voltage Drops

    Directory of Open Access Journals (Sweden)

    Min Ji

    2016-01-01

    Full Text Available Many applications show that semisupervised community detection is one of the important topics and has attracted considerable attention in the study of complex network. In this paper, based on notion of voltage drops and discrete potential theory, a simple and fast semisupervised community detection algorithm is proposed. The label propagation through discrete potential transmission is accomplished by using voltage drops. The complexity of the proposal is OV+E for the sparse network with V vertices and E edges. The obtained voltage value of a vertex can be reflected clearly in the relationship between the vertex and community. The experimental results on four real networks and three benchmarks indicate that the proposed algorithm is effective and flexible. Furthermore, this algorithm is easily applied to graph-based machine learning methods.

  8. Head-on collision of drops: A numerical investigation

    Science.gov (United States)

    Nobari, M. R.; Jan, Y.-J.; Tryggvason, G.

    1993-01-01

    The head-on collision of equal sized drops is studied by full numerical simulations. The Navier-Stokes equations are solved for fluid motion both inside and outside the drops using a front tracking/finite difference technique. The drops are accelerated toward each other by a body force that is turned off before the drops collide. When the drops collide, the fluid between them is pushed outward leaving a thin later bounded by the drop surface. This layer gets progressively thinner as the drops continue to deform and in several of the calculations this double layer is artificially removed once it is thin enough, thus modeling rupture. If no rupture takes place, the drops always rebound, but if the film is ruptured the drops may coalesce permanently or coalesce temporarily and then split again.

  9. Drag and Drop API v HTML5

    OpenAIRE

    BARABÁŠ, Vít

    2013-01-01

    The work (the bachelor´s thesis) deals with a new way of web application management via the "drag and drop" technique in the HTML5 programming language. The work is divided into two parts. The first part consists of DND API description in HTML5. The support analysis within common web browsers is included as a part of this description. The second, practical part of the thesis focuses on a concept and the following realisation of a photogallery using DND API.

  10. Superheated drop as a neutron spectrometer

    OpenAIRE

    Das, Mala; Chatterjee, B. K.; Roy, B.; Roy, S. C.

    2000-01-01

    Superheated drops are known to vaporise when exposed to energetic nuclear radiation since the discovery of bubble chamber. As the degree of superheat increases in a given liquid, less and less energetic neutrons are required to cause nucleation. This property of superheated liquids are being utilised to develope the neutron spectromer. A new principle of neutron spectrometry using Superheated liquid are developed and the developed principle has been tested by Am-Be neutron source.

  11. Low-Pressure-Drop Shutoff Valve

    Science.gov (United States)

    Thornborrow, John

    1994-01-01

    Flapper valve remains open under normal flow conditions but closes upon sudden increases to high rate of flow and remains closed until reset. Valve is fluid/mechanical analog of electrical fuse or circuit breaker. Low-pressure-drop shutoff valve contains flapper machined from cylindrical surface. During normal flow conditions, flapper presents small cross section to flow. (Useful in stopping loss of fluid through leaks in cooling systems.)

  12. Drops on hydrophobic surfaces & vibrated fluid surfaces

    DEFF Research Database (Denmark)

    Wind-Willassen, Øistein

    of a droplet is then given, after which we set up a 2D computational Finite-Element Method (FEM) model for a neutrally buoyant drop immersed in another liquid. The model is validated by considering the volume loss over time. Subsequent to an introduction to the physics of wetting, the developed FEM model......-leap dynamics, exotic trajectories and the emergence of statistical behavior when the forcing is near the Faraday threshold....

  13. The jet mass distribution after Soft Drop

    Science.gov (United States)

    Marzani, Simone; Schunk, Lais; Soyez, Gregory

    2018-02-01

    We present a first-principle computation of the mass distribution of jets which have undergone the grooming procedure known as Soft Drop. This calculation includes the resummation of the large logarithms of the jet mass over its transverse momentum, up to next-to-logarithmic accuracy, matched to exact fixed-order results at next-to-leading order. We also include non-perturbative corrections obtained from Monte-Carlo simulations and discuss analytic expressions for hadronisation and Underlying Event effects.

  14. Eye-Drops for Activation of DREADDs

    Directory of Open Access Journals (Sweden)

    William T. Keenan

    2017-11-01

    Full Text Available Designer Receptors Exclusively Activated by Designer Drugs (DREADDs are an important tool for modulating and understanding neural circuits. Depending on the DREADD system used, DREADD-targeted neurons can be activated or repressed in vivo following a dose of the DREADD agonist clozapine-N-oxide (CNO. Because DREADD experiments often involve behavioral assays, the method of CNO delivery is important. Currently, the most common delivery method is intraperitoneal (IP injection. IP injection is both a fast and reliable technique, but it is painful and stressful particularly when many injections are required. We sought an alternative CNO delivery paradigm, which would retain the speed and reliability of IP injections without being as invasive. Here, we show that CNO can be effectively delivered topically via eye-drops. Eye-drops robustly activated DREADD-expressing neurons in the brain and peripheral tissues and does so at the same dosages as IP injection. Eye-drops provide an easier, less invasive and less stressful method for activating DREADDs in vivo.

  15. Drop friction on liquid-infused surfaces

    Science.gov (United States)

    Gas, Armelle; Keiser, Ludovic; Clanet, Christophe; Quere, David

    2017-11-01

    Trapping a thin liquid film in the roughness of a textured material creates a surface that is partially solid and partially liquid, referred to as a lubricant-impregnated surface. Those surfaces have recently raised a great interest for their promising industrial applications. Indeed, they proved to drastically reduce adhesion of a broad range of liquids, leading to enhanced mobility, and strong anti-biofouling, anti-icing and anti-fogging properties. In our talk we discuss the nature of the friction generated as a drop glides on a textured material infused by another liquid. Different regimes are observed, depending on the viscosities of both liquids. While a viscous drop is simply opposed by a Stokes-type friction, the force opposing a drop moving on a viscous substrate becomes non-linear in velocity. A liquid on an infused material is surrounded by a meniscus, and this specific feature is proposed to be responsible for the special observed frictions, on both adhesive and nonadhesive substrates.

  16. Organization of microbeads in Leidenfrost drops.

    Science.gov (United States)

    Maquet, Laurent; Colinet, Pierre; Dorbolo, Stéphane

    2014-06-21

    We investigated the organization of micrometric hydrophilic beads (glass or basalt) immersed in Leidenfrost drops. Starting from a large volume of water compared to the volume of the beads, while the liquid evaporates, we observed that the grains are eventually trapped at the interface of the droplet and accumulate. At a moment, the grains entirely cover the droplet. We measured the surface area at this moment as a function of the total mass of particles inserted in the droplet. We concluded that the grains form a monolayer around the droplet assuming (i) that the packing of the beads at the surface is a random close packing and (ii) that the initial surface of the drop is larger than the maximum surface that the beads can cover. Regarding the evaporation dynamics, the beads are found to reduce the evaporation rate of the drop. The slowdown of the evaporation is interpreted as being the consequence of the dewetting of the particles located at the droplet interface which makes the effective surface of evaporation smaller. As a matter of fact, contact angles of the beads with the water deduced from the evaporation rates are consistent with contact angles of beads directly measured at a flat air-water interface of water in a container.

  17. Ultrasonic characterization of single drops of liquids

    Energy Technology Data Exchange (ETDEWEB)

    Sinha, D.N.

    1998-04-14

    Ultrasonic characterization of single drops of liquids is disclosed. The present invention includes the use of two closely spaced transducers, or one transducer and a closely spaced reflector plate, to form an interferometer suitable for ultrasonic characterization of droplet-size and smaller samples without the need for a container. The droplet is held between the interferometer elements, whose distance apart may be adjusted, by surface tension. The surfaces of the interferometer elements may be readily cleansed by a stream of solvent followed by purified air when it is desired to change samples. A single drop of liquid is sufficient for high-quality measurement. Examples of samples which may be investigated using the apparatus and method of the present invention include biological specimens (tear drops; blood and other body fluid samples; samples from tumors, tissues, and organs; secretions from tissues and organs; snake and bee venom, etc.) for diagnostic evaluation, samples in forensic investigations, and detection of drugs in small quantities. 5 figs.

  18. Practical neutron dosimetry with superheated drops.

    Science.gov (United States)

    Apfel, R E; Lo, Y C

    1989-01-01

    The Superheated Drop Detector (SDD) is a new kind of neutron detector based on the same principle as that of the bubble chamber, except the superheated material is in drop form suspended by a gel or polymer as first described by Apfel (U.S. Patent 4,143,274). Previously, we have developed a theoretical model for the prediction of the threshold neutron energy to nucleate bubbles in our superheated materials and a model for the calculation of the energy dependent response function of SDD. The results of the theoretical calculations agree with the experimental measurements reasonably well. We found the measured response curve of one of our SDDs follows the same trend as the ideal ICRP dose equivalent response curve within 40% for neutrons of energy above 100 keV and within a factor of 10 below 100 keV. Therefore, it is possible to make a rem-response Superheated Drop Detector. We have further calibrated our SDD with 252Cf neutron sources (both bare and D2O moderated). The results are in reasonable agreement with our theoretical predictions, which proves that our model is valid not only for monoenergetic neutrons but also for neutrons from a radioactive source. The principles of operation of our detector, which can be used in neutron dosimetry, area monitoring, and neutron spectrometry, are discussed.

  19. High-Speed Interferometry Under Impacting Drops

    KAUST Repository

    Langley, Kenneth R.

    2017-08-31

    Over the last decade the rapid advances in high-speed video technology, have opened up to study many multi-phase fluid phenomena, which tend to occur most rapidly on the smallest length-scales. One of these is the entrapment of a small bubble under a drop impacting onto a solid surface. Here we have gone from simply observing the presence of the bubble to detailed imaging of the formation of a lubricating air-disc under the drop center and its subsequent contraction into the bubble. Imaging the full shape-evolution of the air-disc has required μm and sub-μs space and time resolutions. Time-resolved 200 ns interferometry with monochromatic light, has allowed us to follow individual fringes to obtain absolute air-layer thicknesses, based on the eventual contact with the solid. We can follow the evolution of the dimple shape as well as the compression of the gas. The improved imaging has also revealed new levels of detail, like the nature of the first contact which produces a ring of micro-bubbles, highlighting the influence of nanometric surface roughness. Finally, for impacts of ultra-viscous drops we see gliding on ~100 nm thick rarified gas layers, followed by extreme wetting at numerous random spots.

  20. Multiresidue determination of pesticides from aquatic media using polyaniline nanowires network as highly efficient sorbent for microextraction in packed syringe

    Energy Technology Data Exchange (ETDEWEB)

    Bagheri, Habib, E-mail: bagheri@sharif.edu [Environmental and Bio-Analytical Laboratories, Department of Chemistry, Sharif University of Technology, P.O. Box 11365-9516, Tehran (Iran, Islamic Republic of); Alipour, Noshin; Ayazi, Zahra [Environmental and Bio-Analytical Laboratories, Department of Chemistry, Sharif University of Technology, P.O. Box 11365-9516, Tehran (Iran, Islamic Republic of)

    2012-08-31

    Graphical abstract: Polyaniline nanowires network was prepared using soft template technique and used as sorbent of microextraction in packed syringe for the multiresidue determination of selected analytes from triazine, organochlrorine and organophosphorous pesticides in aqueous samples. Highlights: Black-Right-Pointing-Pointer Polyaniline nanowires network was synthesized using soft template method. Black-Right-Pointing-Pointer The presence of micelles was an important parameter in shaping the growing polymer. Black-Right-Pointing-Pointer The synthesized nanowires showed higher extraction capability in comparison with the bulk polymer. - Abstract: A simple, rapid and sensitive method based on microextraction in packed syringe (MEPS), in combination with gas chromatography-mass spectrometry (GC-MS) was developed. Polyaniline (PANI) nanowires network was synthesized and used as sorbent of MEPS for the multiresidue determination of selected analytes from triazine, organochlrorine and organophosphorous pesticides in aqueous samples. The PANI nanowires network was prepared using soft template technique and its characterization was studied by scanning electron microscopy (SEM). The presence of micelles in this methodology showed to be an important parameter in shaping the growing polymer. Hexadecyltrimethylammonium bromide (HTAB) was used as structure directing agent in PANI preparation procedure and this was led to the formation of nanowires with diameters ranging from 35 nm to 45 nm. The synthesized PANI nanowires network showed higher extraction capability in comparison with the bulk PANI. Important parameters influencing the extraction and desorption processes including desorption solvent, elution volume, draw-eject cycles of sample, draw-eject mode, pH effect and amount of sorbent were optimized. Limits of detection were in the range of 0.07-0.3 ng mL{sup -1} using time scheduled selected ion monitoring (SIM) mode. The linearity of method was in the range from 0

  1. Multiresidue determination of pesticides from aquatic media using polyaniline nanowires network as highly efficient sorbent for microextraction in packed syringe

    International Nuclear Information System (INIS)

    Bagheri, Habib; Alipour, Noshin; Ayazi, Zahra

    2012-01-01

    Graphical abstract: Polyaniline nanowires network was prepared using soft template technique and used as sorbent of microextraction in packed syringe for the multiresidue determination of selected analytes from triazine, organochlrorine and organophosphorous pesticides in aqueous samples. Highlights: ► Polyaniline nanowires network was synthesized using soft template method. ► The presence of micelles was an important parameter in shaping the growing polymer. ► The synthesized nanowires showed higher extraction capability in comparison with the bulk polymer. - Abstract: A simple, rapid and sensitive method based on microextraction in packed syringe (MEPS), in combination with gas chromatography–mass spectrometry (GC–MS) was developed. Polyaniline (PANI) nanowires network was synthesized and used as sorbent of MEPS for the multiresidue determination of selected analytes from triazine, organochlrorine and organophosphorous pesticides in aqueous samples. The PANI nanowires network was prepared using soft template technique and its characterization was studied by scanning electron microscopy (SEM). The presence of micelles in this methodology showed to be an important parameter in shaping the growing polymer. Hexadecyltrimethylammonium bromide (HTAB) was used as structure directing agent in PANI preparation procedure and this was led to the formation of nanowires with diameters ranging from 35 nm to 45 nm. The synthesized PANI nanowires network showed higher extraction capability in comparison with the bulk PANI. Important parameters influencing the extraction and desorption processes including desorption solvent, elution volume, draw–eject cycles of sample, draw–eject mode, pH effect and amount of sorbent were optimized. Limits of detection were in the range of 0.07–0.3 ng mL −1 using time scheduled selected ion monitoring (SIM) mode. The linearity of method was in the range from 0.5–200 ng mL −1 to 0.2–1000 ng mL −1 . The method precision

  2. Determination of styrene content in Gorgonzola PDO cheese by headspace solid phase micro-extraction (HS-SPME) and gas-chromatography mass-spectrometry (GC-MS).

    Science.gov (United States)

    Chiesa, L M; Panseri, S; Soncin, S; Vallone, L; Dragoni, I

    2010-06-01

    Control of the composition of products that are intended for use as packaging material is essential, particularly when these products come into direct contact with food. It is well known that plastics are not inert and that their residual monomers, starting substances, and additives are able to migrate into the food they contact. Among plastics, styrene is a common compound found in many plastic containers that can also be produced by the oxidation of Penicillium roqueforti used in gorgonzola Protected Denomination of Origin cheese manufacturing. Therefore, solid-phase microextraction combined with gas chromatography/mass spectrometry was applied in the present work to determine the styrene content in packaged and unpackaged gorgonzola cheese samples to understand styrene migration phenomena from plastic containers.

  3. Low Density Solvent-Based Dispersive Liquid-Liquid Microextraction for the Determination of Synthetic Antioxidants in Beverages by High-Performance Liquid Chromatography

    Science.gov (United States)

    Çabuk, Hasan; Köktürk, Mustafa

    2013-01-01

    A simple and efficient method was established for the determination of synthetic antioxidants in beverages by using dispersive liquid-liquid microextraction combined with high-performance liquid chromatography with ultraviolet detection. Butylated hydroxy toluene, butylated hydroxy anisole, and tert-butylhydroquinone were the antioxidants evaluated. Experimental parameters including extraction solvent, dispersive solvent, pH of sample solution, salt concentration, and extraction time were optimized. Under optimal conditions, the extraction recoveries ranged from 53 to 96%. Good linearity was observed by the square of correlation coefficients ranging from 0.9975 to 0.9997. The relative standard deviations ranged from 1.0 to 5.2% for all of the analytes. Limits of detection ranged from 0.85 to 2.73 ng mL−1. The method was successfully applied for determination of synthetic antioxidants in undiluted beverage samples with satisfactory recoveries. PMID:23853535

  4. Low Density Solvent-Based Dispersive Liquid-Liquid Microextraction for the Determination of Synthetic Antioxidants in Beverages by High-Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Hasan Çabuk

    2013-01-01

    Full Text Available A simple and efficient method was established for the determination of synthetic antioxidants in beverages by using dispersive liquid-liquid microextraction combined with high-performance liquid chromatography with ultraviolet detection. Butylated hydroxy toluene, butylated hydroxy anisole, and tert-butylhydroquinone were the antioxidants evaluated. Experimental parameters including extraction solvent, dispersive solvent, pH of sample solution, salt concentration, and extraction time were optimized. Under optimal conditions, the extraction recoveries ranged from 53 to 96%. Good linearity was observed by the square of correlation coefficients ranging from 0.9975 to 0.9997. The relative standard deviations ranged from 1.0 to 5.2% for all of the analytes. Limits of detection ranged from 0.85 to 2.73 ng mL−1. The method was successfully applied for determination of synthetic antioxidants in undiluted beverage samples with satisfactory recoveries.

  5. Speciation of mercury compounds by gas chromatography with atomic emission detection. Simultaneous optimization of a headspace solid-phase microextraction and derivatization procedure by use of chemometric techniques

    Energy Technology Data Exchange (ETDEWEB)

    Carro, A.M.; Neira, I.; Rodil, R.; Lorenzo, R. A. [Univ. Santiago de Compostela (Spain). Dpto. Quimica Analitica, Nutricion y Bromatologia

    2003-06-01

    A method is proposed for the extraction and determination of organomercury compounds and Hg(II) in seawater samples by headspace solid-phase microextraction (HS-SPME) combined with capillary gas chromatography-microwave-induced plasma atomic emission spectrometry. The mercury species were derivatized with sodium tetraphenylborate, sorbed on a polydimethylsiloxane-coated fused-silica fibre, and desorbed in the injection port of the GC, in splitless mode. Experimental design methodology was used to evaluate the effect of six HS-SPME-derivatization variables: sample volume, NaBPh{sub 4} volume, pH, sorption time, extraction-derivatization temperature, and rate of stirring. Use of a multicriterion decision-making approach, with the desirability function, enabled determination of the optimum working conditions of the procedure for simultaneous analysis of three mercury species. (orig.)

  6. Vortex-assisted surfactant-enhanced emulsification liquid-liquid microextraction for the determination of carbamates in juices by micellar electrokinetic chromatography tandem mass spectrometry.

    Science.gov (United States)

    Moreno-González, David; Huertas-Pérez, José F; García-Campaña, Ana M; Gámiz-Gracia, Laura

    2015-07-01

    A new method based on vortex-assisted surfactant-enhanced-emulsification liquid-liquid microextraction has been developed for the extraction of carbamate pesticides in juice samples prior to their determination by micellar electrokinetic chromatography coupled to tandem mass spectrometry. This sample treatment allowed the satisfactory extraction and the extract clean-up of 25 carbamates from different fruit and vegetal juices (banana, tomato, and peach). In this study, the addition of ammonium perfluorooctanoate in the aqueous sample in combination with vortex agitation, provided very clean extracts with short extraction times. Under optimized conditions, recoveries of the proposed method for these pesticides from fortified juice samples ranged from 81% to 104%, with relative standard deviations lower than 15%. Limits of quantification were between 2.3µgkg(-)(1) and 4.7µgkg(-)(1), showing the high sensitivity of this fast and simple method. Copyright © 2015 Elsevier B.V. All rights reserved.

  7. Determination of Xylene and Toluene by Solid-Phase Microextraction Using Au Nanoparticles-Thiol Silane Film Coupled to Ion Mobility Spectrometry.

    Science.gov (United States)

    Allafchian, Ali Reza; Akhgar, Ava; Ielbeigi, Vahideh; Tabrizchi, Mahmoud

    2016-11-01

    A simple, rapid and sensitive method for analysis of xylene and toluene was developed using the solid-phase microextraction (SPME) combined with ion mobilityspectrometry (IMS). Gold nanoparticles-thiol silane film (Au NPs-TSF) was applied as a newsorbent for SPME. Thiol silane film was formed on the surface of a stainless steel wire through incorporating Au nanoparticles during synthesis using sol-gel technique. The extraction properties of the fiber to xylene and toluene were examined, using a SPME device and thermal desorption ininjection port of IMS. The calibration graphs were linear in the range of 1.10-32.0 and 16.0-112.0 ppb for xylene and toluene, respectively. The detection limits for xylene and toluene were 0.7 and 8.0 ppb, respectively. The proposed method was applied without any considerable sample pretreatment and it was found to be simple enough to be strongly recommended for real sample analysis.

  8. Hollow fiber-based liquid-phase microextraction (HF-LPME) of ibuprofen followed by FIA-chemiluminescence determination using the acidic permanganate-sulfite system.

    Science.gov (United States)

    Payán, María Ramos; López, Miguel Angel Bello; Fernández-Torres, Rut; Navarro, Mercedes Villar; Mochón, Manuel Callejón

    2009-08-15

    Hollow fiber-based liquid-phase microextraction (HF-LPME) is a relatively new technique employed in analytical chemistry for sample pretreatment which offers more selectivity and sensitivity than any traditional extraction technique. This paper describes a three-phase HF-LPME method for ibuprofen using a polypropylene membrane supporting dihexyl ether followed by a chemiluminescence (CL) determination using the CL enhancement on the acidic permanganate-sulfite system in a FIA configuration which is the first time that both techniques have been combined for analytical purposes. The CL intensity (peak area) was proportional to the log of ibuprofen concentration in the donor phase over the range 0.1-20 microg mL(-1). The detection limit was 0.03 microg mL(-1) of ibuprofen in the donor phase. The method was satisfactory reproducible and has been applied to the ibuprofen determination in pharmaceuticals and in real human urine samples.

  9. Capillary migration of large confined super-hydrophobic drops in wedges

    Science.gov (United States)

    Torres, Logan; Weislogel, Mark; Arnold, Sam

    2016-11-01

    When confined within an interior corner, drops and bubbles migrate to regions of minimum energy by the combined effects of surface tension, surface wetting, and corner geometry. Such capillary phenomena are exploited for passive phase separation operations in micro-fluidic devices on earth and macro-fluidic devices aboard spacecraft. Our study focuses on the migration of large inertial-capillary drops confined between two planar super-hydrophobic surfaces. In our experiments, the near weightless environment of a drop tower produces Bo <<1 for drop volumes O(10mL) with migration velocities up to 10 cm/s. We observe transient power law behavior as a function of drop volume, wedge angle, initial confinement, and fluid properties including contact angle. We then further demonstrate how the experiment method may be employed as a large horizontal quiescent droplet generator for studies ranging from inertial non-wetting moving contact line investigations to large geyser-free horizontal drop impacts. NASA Cooperative Agreement NNX12AO47A, URMP.

  10. New approach applying a pet fish air pump in liquid-phase microextraction for the determination of Sudan dyes in food samples by HPLC.

    Science.gov (United States)

    Sricharoen, Phitchan; Limchoowong, Nunticha; Techawongstien, Suchila; Chanthai, Saksit

    2017-10-01

    A new approach applying a pet fish air pump is introduced to develop an extraction method, namely, air-pump-enhanced emulsion, followed by salt-assisted emulsion breaking based on solidified floating organic drop microextraction for the extraction and preconcentration of Sudan I-IV before high-performance liquid chromatography. The applicability of this method was successfully demonstrated by determination of these dyes in four chili products that include chili powder, chili oil, chili sauce, and chili paste. An enrichment factor of 62 was obtained only with a sample solution of 5 mL. A linear range of 0.5-2500 ng/mL was obtained with a limit of detection of 0.16-0.24 ng/mL and recovery of 90-110%. This method is superior to other liquid-liquid extraction methods, as is simple, rapid, environmental friendly, and its phase separation needs no centrifugation. It also needs no disperser solvent and requires less organic solvent, and satisfies the criteria to be called as a green extraction. Therefore, this facile extraction method can be successfully applied in the determination of Sudan dyes in food samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Binary-solvent-based ionic-liquid-assisted surfactant-enhanced emulsification microextraction for the determination of four fungicides in apple juice and apple vinegar.

    Science.gov (United States)

    Chen, Xiaochu; Zhang, Xu; Liu, Fengmao; Hou, Fan

    2017-02-01

    A binary-solvent-based ionic-liquid-assisted surfactant-enhanced emulsification microextraction method was developed for the separation/preconcentration and determination of four fungicides (pyrimethanil, fludioxonil, cyprodynil, pyraclostrobin) in apple juice and apple vinegar. A nonchlorinated solvent amyl acetate, which has a lower density than water, was used as the extraction solvent, and an ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate, which has a high density and low toxicity, was used as a secondary solvent mixed with the extraction solvent. After centrifugation, the binary solvent drop with a relatively high density was deposited on the bottom of the tube. Some parameters influencing the extraction efficiency of analytes such as type of extraction solvent, ratio of ionic liquid, volume of mixed solvent, type and concentration of surfactant, sample pH, NaCl concentration, and vortex time were investigated and optimized. Under the optimized conditions, the proposed method provided a good linearity in the range of 5-200 μg/L. The limits of quantification of the method were in the range of 2-5 μg/L. The relative standard deviations for interday assays were 1.7-11.9%. The method was applied to the determination of pyrimethanil, fludioxonil, cyprodynil, and pyraclostrobin in apple juice and apple vinegar samples, and the accuracy was evaluated through recovery experiments. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Dispersive liquid-liquid microextraction based on solidification of floating organic droplet for the determination of triazine and triazoles in mineral water samples.

    Science.gov (United States)

    Bolzan, Cátia M; Caldas, Sergiane S; Guimarães, Bruno S; Primel, Ednei G

    2016-09-01

    A simple, rapid, and sensitive method for the determination of atrazine, simazine, cyproconazole, tebuconazole, and epoxiconazole in mineral water employing the dispersive liquid-liquid microextraction with solidification of a floating organic drop with determination by liquid chromatography tandem mass spectrometry has been developed. A mixed solution of 250 μL 1-dodecanol and 1250 μL methanol was injected rapidly into 10 mL aqueous solution (pH 7.0) with 2% w/v NaCl. After centrifugation for 5 min at 2000 rpm, the organic solvent droplets floated on the surface of the aqueous solution and the floating solvent solidified. The method limits of detection were between 3.75 and 37.5 ng/L and limits of quantification were between 12.5 and 125 ng/L. The recoveries ranged from 70 to 118% for repeatability and between 76 and 95% for intermediate precision with a relative standard deviation from 2 to 18% for all compounds. Low matrix effect was observed. The proposed method can be successfully applied in routine analysis for determination of pesticide residues in mineral water samples, allowing for monitoring of triazine and triazoles at levels below the regulatory limits set by international and national legislations. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Laplacian drop shapes and effect of random perturbations on accuracy of surface tension measurement for different drop constellations.

    Science.gov (United States)

    Saad, Sameh M I; Neumann, A Wilhelm

    2015-08-01

    Theoretical drop shapes are calculated for three drop constellations: pendant drops, constrained sessile drops, and unconstrained sessile drops. Based on total Gaussian curvature, shape parameter and critical shape parameter are discussed as a function of different drop sizes and surface tensions. The shape parameter is linked to physical parameters for every drop constellation. The as yet unavailable detailed dimensional analysis for the unconstrained sessile drop is presented. Results show that the unconstrained sessile drop shape depends on a dimensionless volume term and the contact angle. Random perturbations are introduced and the accuracy of surface tension measurement is assessed for precise and perturbed profiles of the three drop constellations. It is concluded that pendant drops are the best method for accurate surface tension measurement, followed by constrained sessile drops. The unconstrained sessile drops come last because they tend to be more spherical at low and moderate contact angles. Of course, unconstrained sessile drops are the only option if contact angles are to be measured. Copyright © 2014 Elsevier B.V. All rights reserved.

  14. Magnetical hollow fiber bar collection of extract in homogenous ionic liquid microextraction of triazine herbicides in water samples.

    Science.gov (United States)

    Wang, Kun; Jiang, Jia; Kang, Mingqin; Li, Dan; Zang, Shuang; Tian, Sizhu; Zhang, Hanqi; Yu, Aimin; Zhang, Ziwei

    2017-04-01

    The homogeneous ionic liquid microextraction combined with magnetical hollow fiber bar collection was developed for extracting triazine herbicides from water samples. These analytes were separated and determined by high performance liquid chromatography. The triazines were quickly extracted into ionic liquid microdroplets dispersed in solution, and then these microdroplets were completely collected with magnetical hollow fiber bars; the pores of which were impregnated with hydrophobic ionic liquid, which makes the phase separation simplified with no need of centrifugation. Some experimental parameters, such as the type of ionic liquid, ultrasonic immersion time of hollow fiber, pH of sample solution, volume of hydrophilic ionic liquid, amount of ion-pairing agent NH 4 PF 6 , NaCl concentration, number of magnetical hollow fiber bar, stirring rate, and collection time were investigated and optimized. When the present method was applied to the analysis of real water samples, the precision and recoveries of six triazine herbicides vary from 0.1 to 9.2% and 73.4 to 118.5%, respectively. The detection limits for terbumeton, ametryn, prometryn, terbutryn, trietazine, and dimethametryn were 0.48, 0.15, 0.15, 0.14, 0.35, and 0.16 μg L -1 , respectively.

  15. Characterization of volatile compounds in fermented milk using solid-phase microextraction methods coupled with gas chromatography-mass spectrometry.

    Science.gov (United States)

    Dan, T; Wang, D; Jin, R L; Zhang, H P; Zhou, T T; Sun, T S

    2017-04-01

    Lactic acid bacteria (LAB) are industrially important bacteria that are widely used in the fermented food industry, especially in the manufacture of yogurt. Characteristic flavors are produced by LAB during fermentation and storage that affect the quality and acceptability of fermented milk products. In this study, the volatile compounds in milk fermented by Streptococcus thermophilus IMAU80842 alone, Lactobacillus delbrueckii ssp. bulgaricus IMAU20401 alone, or both species together were identified using solid-phase microextraction methods coupled with gas chromatography-mass spectrometry. A total of 53, 43, and 32 volatile compounds were identified in milk fermented by S. thermophilus alone, L. delbrueckii ssp. bulgaricus alone, or both species together, respectively. The presence of some important flavor compounds was confirmed: acetic acid, acetaldehyde, acetoin, 2,3-butanedione, ethanol, and 1-heptanol. Our results demonstrate that the composition of the volatile compounds in fermented milk depends on the species of LAB used and whether they are used alone or in combination. This is important for the selection of appropriate starter cultures for the production of different types of fermented milk product with particular flavors. Copyright © 2017 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

  16. Improving the Sensitivity of Solid-Phase Microextraction by Reducing the Volume of Off-Line Elution Solvent.

    Science.gov (United States)

    Xu, Jianqiao; Liu, Xiwen; Wang, Qi; Huang, Shuyao; Yin, Li; Xu, Jing; Liu, Xianguo; Jiang, Ruifen; Zhu, Fang; Ouyang, Gangfeng

    2018-02-06

    Solid-phase microextraction (SPME) coupled with liquid chromatograph (LC) is widely used to detect polar and ionic organic compounds, including various pharmaceuticals and endogenous bioactive compounds. In this study, a small-sized insert tube for use in the commercial autosampler vial was designed for eluting the extracted analytes from SPME fibers for LC analysis. By using this custom-made insert tube as an alternative to the commercial insert tube, the volume of the elution solvent was reduced by four-fifths. Even though smaller fractions of the analytes were eluted from the fiber coatings, the analyte concentrations in the elution solutions were substantially increased by using the custom-made insert tube. Therefore, larger amounts of the analytes could be injected to LC and higher signal-to-noise ratios could be achieved, even at smaller injection volumes. Since the elution in the custom-made insert tube was nonexhaustive, four strategies were developed to figure out the extracted amounts in the fiber coatings. In combination with the sampling-rate calibration method, these strategies were successfully used to determine the concentrations of fluoxetine in living tilapias. This study provides a simple but effect way for improving the analytical sensitivity when coupling SPME with LC.

  17. Determination of polycyclic aromatic hydrocarbons in fresh milk by hollow fiber liquid-phase microextraction-gas chromatography mass spectrometry.

    Science.gov (United States)

    Sanagi, Mohd Marsin; Loh, Saw Hong; Wan Ibrahim, Wan Aini; Hasan, Mohamed Noor; Aboul Enein, Hassan Y

    2013-02-01

    In this work, a two-phase hollow fiber liquid-phase microextraction (HF-LPME) method combined with gas chromatography-mass spectrometry (GC-MS) is developed to provide a rapid, selective and sensitive analytical method to determine polycyclic aromatic hydrocarbons (PAHs) in fresh milk. The standard addition method is used to construct calibration curves and to determine the residue levels for the target analytes, fluorene, phenanthrene, fluoranthene, pyrene and benzo[a]pyrene, thus eliminating sample pre-treatment steps such as pH adjustment. The HF-LPME method shows dynamic linearity from 5 to 500 µg/L for all target analytes with R(2) ranging from 0.9978 to 0.9999. Under optimized conditions, the established detection limits range from 0.07 to 1.4 µg/L based on a signal-to-noise ratio of 3:1. Average relative recoveries for the determination of PAHs studied at 100 µg/L spiking levels are in the range of 85 to 110%. The relative recoveries are slightly higher than those obtained by conventional solvent extraction, which requires saponification steps for fluorene and phenanthrene, which are more volatile and heat sensitive. The HF-LPME method proves to be simple and rapid, and requires minimal amounts of organic solvent that supports green analysis.

  18. In situ derivatization and hollow fiber membrane microextraction for gas chromatographic determination of haloacetic acids in water.

    Science.gov (United States)

    Varanusupakul, Pakorn; Vora-Adisak, Narongchai; Pulpoka, Bancha

    2007-08-13

    An alternative method for gas chromatographic determination of haloacetic acids (HAAs) in water using direct derivatization followed by hollow fiber membrane liquid-phase microextraction (HF-LPME) has been developed. The method has improved the sample preparation step according to the conventional US EPA Method 552.2 by combining the derivatization and the extraction into one step prior to determination by gas chromatography electron captured detector (GC-ECD). The HAAs were derivatized with acidic methanol into their methyl esters and simultaneously extracted with supported liquid hollow fiber membrane in headspace mode. The derivatization was attempted directly in water sample without sample evaporation. The HF-LPME was performed using 1-octanol as the extracting solvent at 55 degrees C for 60 min with 20% Na2SO4. The linear calibration curves were observed for the concentrations ranging from 1 to 300 microg L(-1) with the correlation coefficients (R2) being greater than 0.99. The method detection limits of most analytes were below 1 microg L(-1) except DCAA and MCAA that were 2 and 18 microg L(-1), respectively. The recoveries from spiked concentration ranged from 97 to 109% with %R.S.D. less than 12%. The method was applied for determination of HAAs in drinking water and tap water samples. The method offers an easy one step high sample throughput sample preparation for gas chromatographic determination of haloacetic acids as well as other contaminants in water.

  19. Identification and quantification of organic pollutants in the air of the city of Astana using solid phase microextraction

    Directory of Open Access Journals (Sweden)

    Dina Orazbayeva

    2017-06-01

    Full Text Available Solid-phase microextraction in combination with gas chromatography and mass-spectrometry (GC-MS was used for determination of benzene, toluene, ethylbenzene and o-xylene (BTEX, polycyclic aromatic hydrocarbons (PAH, and for identification of volatile organic compounds (VOCs in ambient air of the city of Astana, Kazakhstan. The screening of the samples showed the presence of mono- and polycyclic aromatic hydrocarbons, alkanes, alkenes, phenols, and benzaldehydes. The concentrations of naphthalene were 5-7 times higher than the permissible value, it was detected in all studied air samples. Average concentration of naphthalene was 18.4 μg/m3, acenaphthylene – 0.54 μg/m3, acenaphthene – 1.63 μg/m3, fluorene – 0.79 μg/m3, anthracene – 3.27 μg/m3, phenanthrene – 0.22 μg/m3, fluorantene – 0.74 μg/m3, pyrene – 0.73 μg/m3. Average concentrations of BTEX in the studied samples were 31.1, 84.9, 10.8 and 11.6 μg/m3, respectively. Based on the statistical analysis of the concentrations of BTEX and PAH, the main source of city air pollution with them was assumed to be vehicle emissions.

  20. Surfactant-enhanced liquid-liquid microextraction coupled to micro-solid phase extraction onto highly hydrophobic magnetic nanoparticles

    International Nuclear Information System (INIS)

    Giannoulis, Kiriakos M.; Giokas, Dimosthenis L.; Tsogas, George Z.; Vlessidis, Athanasios G.; Zhu, Qing; Pan, Qinmin

    2013-01-01

    We are presenting a simplified alternative method for dispersive liquid-liquid microextraction (DLLME) by resorting to the use of surfactants as emulsifiers and micro solid-phase extraction (μ-SPE). In this combined procedure, DLLME of hydrophobic components is initially accomplished in a mixed micellar/microemulsion extractant phase that is prepared by rapidly mixing a non-ionic surfactant and 1-octanol in aqueous medium. Then, and in contrast to classic DLLME, the extractant phase is collected by highly hydrophobic polysiloxane-coated core-shell Fe 2 O 3 (at)C magnetic nanoparticles. Hence, the sample components are the target analyte in the DLLME which, in turn, becomes the target analyte of the μ-SPE step. This 2-step approach represents a new and simple DLLME procedure that lacks tedious steps such as centrifugation, thawing, or delicate collection of the extractant phase. As a result, the analytical process is accelerated and the volume of the collected phase does not depend on the volume of the extraction solvent. The method was applied to extract cadmium in the form of its pyrrolidine dithiocarbamate chelate from spiked water samples prior to its determination by FAAS. Detection limits were brought down to the low μg L −1 levels by preconcentrating 10 mL samples with satisfactory recoveries (96.0–108.0 %). (author)

  1. In situ derivatization and hollow fiber membrane microextraction for gas chromatographic determination of haloacetic acids in water

    International Nuclear Information System (INIS)

    Varanusupakul, Pakorn; Vora-adisak, Narongchai; Pulpoka, Bancha

    2007-01-01

    An alternative method for gas chromatographic determination of haloacetic acids (HAAs) in water using direct derivatization followed by hollow fiber membrane liquid-phase microextraction (HF-LPME) has been developed. The method has improved the sample preparation step according to the conventional US EPA Method 552.2 by combining the derivatization and the extraction into one step prior to determination by gas chromatography electron captured detector (GC-ECD). The HAAs were derivatized with acidic methanol into their methyl esters and simultaneously extracted with supported liquid hollow fiber membrane in headspace mode. The derivatization was attempted directly in water sample without sample evaporation. The HF-LPME was performed using 1-octanol as the extracting solvent at 55 deg. C for 60 min with 20% Na 2 SO 4 . The linear calibration curves were observed for the concentrations ranging from 1 to 300 μg L -1 with the correlation coefficients (R 2 ) being greater than 0.99. The method detection limits of most analytes were below 1 μg L -1 except DCAA and MCAA that were 2 and 18 μg L -1 , respectively. The recoveries from spiked concentration ranged from 97 to 109% with %R.S.D. less than 12%. The method was applied for determination of HAAs in drinking water and tap water samples. The method offers an easy one step high sample throughput sample preparation for gas chromatographic determination of haloacetic acids as well as other contaminants in water

  2. Quantification of synthetic organic chemicals in biological treatment process effluent using solid-phase microextraction and gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Magbanua, B.S. Jr.; Mitchell, D.R.; Fehniger, S.M.; Bowyer, R.L.; Grady, C.P.L. Jr.

    2000-02-01

    Solid-phase microextraction (SPME), a technique that uses a polymer-coated, fused-silica fiber to selectively extract organic analyses from a sample matrix, followed by gas chromatography (GC), was used to quantify selected synthetic organic chemicals (SOCs) in biological reactor effluent. By selecting an appropriate combination of SPME fiber, GC column, and GC detector, assays to quantify either a suite of SOCs or single selected SOCs were developed. Phenol, 4-chlorophenol, 2-nitrophenol, 4-nitrophenol, 2,4,-dinitrophenol, isophorone, m-toluate, m-sylene, and di-n-butylphthalate were quantified simultaneously using an 85-{micro}m polyacrylate SPME fiber, a 5% diphenyl-95% dimethyl polysiloxane capillary column, and a flame ionization detector. m-Xylene was quantified using a 100-{micro}m polydimethylsiloxane SPME fiber, a 5% diphenyl-95% dimethyl polysiloxane capillary column, and a mass spectrometric detector. Dichloromethane was quantified using an 85-{micro}m polyacrylate SPME fiber, a Carbopack B/1% SP-1000 packed column, and an electron capture detector. All three assays enabled detection of the target analyses to low concentrations ({micro}g/L) with minimal sample volume and processing requirements.

  3. Rapid Separation of Elemental Species by Fast Multicapillary Gas Chromatography with Multichannel Optical Spectrometry Detection following Headspace Solid Phase Microextraction

    Directory of Open Access Journals (Sweden)

    Jacek Giersz

    2015-05-01

    Full Text Available A method for conducting fast and efficient gas chromatography based on short multicapillaries in straight alignment combined with atomic emission detection was developed for field analysis. The strategy enables for speciation analysis of organometallic compounds. The analytes are simultaneously ethylated and preconcentrated on a solid phase microextraction (SPME fiber placed in the headspace over the sample for 25 min. The ethylated species are then completely separated and selectively quantified within 25 s under isothermal conditions. A new miniaturized speciation analyzer has been constructed and evaluated. The system consists of a GC injection port and a lab-made miniaturized GC unit directly coupled with miniaturized plasma excitation source. The emitted light is transferred via optical fiber and registered with a miniaturized charged coupled device (CCD based spectrometer. Working parameters for multicapillary column gas chromatography with atomic emission detector, including carrier gas flow rate, desorption temperature, and GC column temperature, were optimized to achieve good separation of analytes. Basic investigations of the fundamental properties of 5 cm-long multicapillary column, to evaluate its potential and limitations as a rapid separation unit, are presented. The adaptation of the technique for use with a SPME system and with a multichannel element-selective plasma-emission detector is highlighted.

  4. An Effective Method to Detect Volatile Intermediates Generated in the Bioconversion of Coal to Methane by Gas Chromatography-Mass Spectrometry after In-Situ Extraction Using Headspace Solid-Phase Micro-Extraction under Strict Anaerobic Conditions.

    Science.gov (United States)

    Liu, Jianmin; Wang, Baoyu; Tai, Chao; Wu, Li; Zhao, Han; Guan, Jiadong; Chen, Linyong

    2016-01-01

    Bioconversion of coal to methane has gained increased attention in recent decades because of its economic and environmental advantages. However, the mechanism of this process is difficult to study in depth, partly because of difficulties associated with the analysis of intermediates generated in coal bioconversion. In this investigation, we report on an effective method to analyze volatile intermediates generated in the bioconversion of coal under strict anaerobic conditions. We conduct in-situ extraction of intermediates using headspace solid-phase micro-extraction followed by detection by gas chromatography-mass spectrometry. Bioconversion simulation equipment was modified and combined with a solid-phase micro-extraction device. In-situ extraction could be achieved by using the combined units, to avoid a breakdown in anaerobic conditions and to maintain the experiment continuity. More than 30 intermediates were identified qualitatively in the conversion process, and the variation in trends of some typical intermediates has been discussed. Volatile organic acids (C2-C7) were chosen for a quantitative study of the intermediates because of their importance during coal bioconversion to methane. Fiber coating, extraction time, and solution acidity were optimized in the solid-phase micro-extraction procedure. The pressure was enhanced during the bioconversion process to investigate the influence of headspace pressure on analyte extraction. The detection limits of the method ranged from 0.0006 to 0.02 mmol/L for the volatile organic acids and the relative standard deviations were between 4.6% and 11.5%. The volatile organic acids (C2-C7) generated in the bioconversion process were 0.01-1.15 mmol/L with a recovery range from 80% to 105%. The developed method is useful for further in-depth research on the bioconversion of coal to methane.

  5. Dispersive liquid-liquid microextraction of phenolic compounds from vegetable oils using a magnetic ionic liquid.

    Science.gov (United States)

    Zhu, Shuqiang; Wang, Lijun; Su, Along; Zhang, Haixia

    2017-08-01

    A novel method was developed for the determination of two endocrine-disrupting chemicals, bisphenol A and 4-nonylphenol, in vegetable oil by dispersive liquid-liquid microextraction followed by ultra high performance liquid chromatography with tandem mass spectrometry. Using a magnetic liquid as the microextraction solvent, several key parameters were optimized, including the type and volume of the magnetic liquid, extraction time, amount of dispersant, and the type of reverse extractant. The detection limits for bisphenol A and 4-nonylphenol were 0.1 and 0.06 μg/kg, respectively. The recoveries were 70.4-112.3%, and the relative standard deviations were less than 4.2%. The method is simple for the extraction of bisphenol A and 4-nonylphenol from vegetable oil and suitable for routine analysis. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Packet Drop Avoidance for High-speed network transmission protocol

    Energy Technology Data Exchange (ETDEWEB)

    Jin, Guojun

    2004-05-01

    As network bandwidth continues to grow and longer paths are used to exchange large scientific data between storage systems and GRID computation, it has become increasingly obvious that there is a need to deploy a packet drop avoidance mechanism into network transmission protocols. Current end-to-end congestion avoidance mechanisms used in Transmission Control Protocol (TCP) have worked well on low bandwidth delay product networks, but with newer high-bandwidth delay networks they have shown to be inefficient and prone to unstable. This is largely due to increased network bandwidth coupled with changes in internet traffic patterns. These changes come from a variety of new network applications that are being developed to take advantage of the increased network bandwidth. This paper will examine the end-to-end congestion avoidance mechanism and perform a step-by-step analysis of its theory. In addition we will propose an alternative approach developed as part of a new network transmission protocol. Our alternative protocol uses a packet drop avoidance (PDA) mechanism built on top of the maximum burst size (MBS) theory combined with a real-time available bandwidth algorithm.

  7. Applications of Liquid-Phase Microextraction in the Sample Preparation of Environmental Solid Samples

    OpenAIRE

    Helena Prosen

    2014-01-01

    Solvent extraction remains one of the fundamental sample preparation techniques in the analysis of environmental solid samples, but organic solvents are toxic and environmentally harmful, therefore one of the possible greening directions is its miniaturization. The present review covers the relevant research from the field of application of microextraction to the sample preparation of environmental solid samples (soil, sediments, sewage sludge, dust etc.) published in the last decade. Several...

  8. Optimization of the solid-phase microextraction method in the determination of Ixodes ricinus (L.) volatiles

    Czech Academy of Sciences Publication Activity Database

    Zahradníčková, Helena; Bouman, Edwin Arien Poul

    2006-01-01

    Roč. 29, č. 2 (2006), s. 236-241 ISSN 1615-9306 R&D Projects: GA ČR(CZ) GA206/04/0751 Institutional research plan: CEZ:AV0Z50070508; CEZ:AV0Z60220518 Keywords : GC/MS * Ixodes ricinus * solid-phase microextraction Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.535, year: 2006

  9. Drying drops : Drying drops containing solutes: From hydrodynamical to mechanical instabilities.

    Science.gov (United States)

    Giorgiutti-Dauphiné, F; Pauchard, L

    2018-03-19

    The drying of complex fluids involves a large number of microscopic phenomena (transport and organization of non-volatile solutes) as well as hydrodynamic and mechanical instabilities. These phenomena can be captured in drying sessile drops where different domains can be identified: strong concentration gradients, formation of a glassy or porous envelope that withstands mechanical stress, and consolidation of a layer strongly adhering to the substrate at the drop edge. In colloidal systems, we quantify the evolution of the particle volume fraction at a nanometric scale and microscopic scale and identify the conditions for the envelope formation at the free surface by balancing the effect of diffusion and evaporation. When a solid envelope is formed at a drop surface, the mechanical instabilities induced by the drying result in different drop shapes. Finally, large drying stresses build up in the solid layer adhering on the substrate, and possibly cause crack formation. In particular, we study how crack patterns are affected by the contact angle of drops and the drying conditions. A particular interest of the review is devoted to drying pattern of solutes.

  10. Simplified procedure for determining of drop and stilling basin

    Directory of Open Access Journals (Sweden)

    Ali R. Vatankhah

    2014-03-01

    Full Text Available Drops are used to effectively dissipate the surplus energy of the water flow. A closed conduit drop conveys water and stills it at its downstream. I-type pipe drop is one kind of the closed conduit drops which is used in irrigation networks as a typical hydraulic structure. Sump elevation is an important design parameter for I-type pipe drop. Similarly, in supercritical flow structures, such as open channel chutes, determination of stilling basin invert elevation is very important. At present, these key design parameters are determined by the momentum and energy equations using tedious trial-and-error procedure. In this study, square conduit drop, pipe drop, and rectangular stilling basin are considered, and three explicit equations have been developed by (multiple nonlinear regression technique to determine the sump and stilling basin invert elevations. Being very simple and accurate, these equations can be easily used to design the closed conduit drops and stilling basins by hydraulic engineers.

  11. Numerical simulation of the combustion process of a pellet-drop-feed boiler

    NARCIS (Netherlands)

    Gómez, M. A.; Porteiro, J.; De la Cuesta de Cal, Daniel; Patiño, D.; Míguez, J. L.

    2016-01-01

    This paper presents a transient model for the simulation of biomass combustion in a fixed bed boiler fed through particle drop. The method combines classical CFD techniques, which are used to simulate the gas phase, with a set of Eulerian variables defined to model the solid phase and Lagrangian

  12. MediaEval 2014: A Multimodal Approach to Drop Detection in Electronic Dance Music

    NARCIS (Netherlands)

    Aljanaki, Anna; Soleymani, Mohammad; Wiering, Frans; Veltkamp, Remco

    2014-01-01

    We predict drops in electronic dance music (EDM), employing different multimodal approaches. We combine three sources of data: noisy labels collected through crowdsourcing, timed comments from SoundCloud and audio content analysis. We predict the correct labels from the noisy labels using the

  13. Rapid ionic liquid-based ultrasound assisted dual magnetic microextraction to preconcentrate and separate cadmium-4-(2-thiazolylazo)-resorcinol complex from environmental and biological samples.

    Science.gov (United States)

    Khan, Sumaira; Kazi, Tasneem Gul; Soylak, Mustafa

    2014-04-05

    A rapid and innovative microextraction technique named as, ionic liquid-based ultrasound-assisted dual magnetic microextraction (IL-UA-DMME) was developed for the preconcentration and extraction of trace cadmium from environmental and biological samples, prior to analyzed by flame atomic absorption spectrometry (FAAS). The proposed method has many obvious advantages, including evading the use of organic solvents and achieved high extraction yields by the combination of dispersive liquid-liquid microextraction (DLLME) and magnetic mediated-solid phase extraction (MM-SPE). In this approach ionic liquid (IL) 1-butyl-3-methylimidazolium hexafluorophosphate [C4mim][PF6] play an important role to extract the cadmium-4-(2-thiazolylazo)-resorcinol (Cd-TAR) complex from acid digested sample solutions and ultrasonic irradiation was applied to assist emulsification. After then, dispersed small amount of Fe3O4 magnetic nanoparticles (MNPs) in sample solutions to salvaged the IL and complete phase separation was attained. Some analytical parameters that influencing the efficiency of proposed (IL-UA-DMME) method, such as pH, volume of IL, ligand concentration, ultra-sonication time, amount of Fe3O4 MNPs, sample volume and matrix effect were optimized. Limit of detection (LOD) and enrichment factor (EF) of the method under optimal experimental conditions were found to be 0.40μgL(-1) and 100, respectively. The relative standard deviation (RSD) of 50μgL(-1) Cd was 4.29%. The validity and accuracy of proposed method, was assessed to analyzed certified reference materials of fortified lake water TMDA-54.4, SPS-WW2 waste water, spinach leaves 1570a and also checked by standard addition method. The obtained values showed good agreement with the certified values and sufficiently high recovery were found in the range of 98.1-101% for Cd. The proposed method was facile, rapid and successfully applied for the determination of Cd in environmental and different biological samples

  14. On-line electrochemically controlled in-tube solid phase microextraction of inorganic selenium followed by hydride generation atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Asiabi, Hamid [Department of Chemistry, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of); Yamini, Yadollah, E-mail: yyamini@modares.ac.ir [Department of Chemistry, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of); Seidi, Shahram [Department of Analytical Chemistry, Faculty of Chemistry, K.N. Toosi University of Technology, Tehran (Iran, Islamic Republic of); Shamsayei, Maryam; Safari, Meysam; Rezaei, Fatemeh [Department of Chemistry, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of)

    2016-05-30

    In this work, for the first time, a rapid, simple and sensitive microextraction procedure is demonstrated for the matrix separation, preconcentration and determination of inorganic selenium species in water samples using an electrochemically controlled in-tube solid phase microextraction (EC-in-tube SPME) followed by hydride generation atomic absorption spectrometry (HG-AAS). In this approach, in which EC-in-tube SPME and HG-AAS system were combined, the total analysis time, was decreased and the accuracy, repeatability and sensitivity were increased. In addition, to increases extraction efficiency, a novel nanostructured composite coating consisting of polypyrrole (PPy) doped with ethyleneglycol dimethacrylate (EGDMA) was prepared on the inner surface of a stainless-steel tube by a facile electrodeposition method. To evaluate the offered setup and the new PPy-EGDMA coating, it was used to extract inorganic selenium species in water samples. Extraction of inorganic selenium species was carried out by applying a positive potential through the inner surface of coated in-tube under flow conditions. Under the optimized conditions, selenium was detected in amounts as small as 4.0 parts per trillion. The method showed good linearity in the range of 0.012–200 ng mL{sup −1}, with coefficients of determination better than 0.9996. The intra- and inter-assay precisions (RSD%, n = 5) were in the range of 2.0–2.5% and 2.7–3.2%, respectively. The validated method was successfully applied for the analysis of inorganic selenium species in some water samples and satisfactory results were obtained. - Graphical abstract: An electrochemically controlled in-tube solid phase microextraction followed by hydride generation atomic absorption spectrometry was developed for extraction and determination ultra-trace amounts of Se in aqueous solutions. - Highlights: • A nanostructured composite coating consisting of PPy doped with EGDMA was prepared. • The coating was

  15. Partial coalescence from bubbles to drops

    KAUST Repository

    Zhang, F. H.

    2015-10-07

    The coalescence of drops is a fundamental process in the coarsening of emulsions. However, counter-intuitively, this coalescence process can produce a satellite, approximately half the size of the original drop, which is detrimental to the overall coarsening. This also occurs during the coalescence of bubbles, while the resulting satellite is much smaller, approximately 10 %. To understand this difference, we have conducted a set of coalescence experiments using xenon bubbles inside a pressure chamber, where we can continuously raise the pressure from 1 up to 85 atm and thereby vary the density ratio between the inner and outer fluid, from 0.005 up to unity. Using high-speed video imaging, we observe a continuous increase in satellite size as the inner density is varied from the bubble to emulsion-droplet conditions, with the most rapid changes occurring as the bubble density grows up to 15 % of that of the surrounding liquid. We propose a model that successfully relates the satellite size to the capillary wave mode responsible for its pinch-off and the overall deformations from the drainage. The wavelength of the primary wave changes during its travel to the apex, with the instantaneous speed adjusting to the local wavelength. By estimating the travel time of this wave mode on the bubble surface, we also show that the model is consistent with the experiments. This wavenumber is determined by both the global drainage as well as the interface shapes during the rapid coalescence in the neck connecting the two drops or bubbles. The rate of drainage is shown to scale with the density of the inner fluid. Empirically, we find that the pinch-off occurs when 60 % of the bubble fluid has drained from it. Numerical simulations using the volume-of-fluid method with dynamic adaptive grid refinement can reproduce these dynamics, as well as show the associated vortical structure and stirring of the coalescing fluid masses. Enhanced stirring is observed for cases with second

  16. Study of eye drops dispensing and dose variability by using plastic dropper tips.

    Science.gov (United States)

    Sklubalová, Zdenka; Zatloukal, Zdenek

    2006-02-01

    The application of eye drops from flexible dropper bottles fitted with different types of dropper tips is associated with the high variability of eye drop weights. The aim of this report was to investigate the simultaneous effect of three factors influencing the mean weight of drops dispensing from two plastic dropper tips. Using a designed experiment (Box-Behnken), the effect of the concentration of benzalkonium chloride solutions (BAC) in the range of 0-0.02%, the dispensing angle from 90 degrees to 30 degrees from horizontal, and the residual volume of liquid in the dropper bottle from 4 to 10 mL on the mean drop weights were examined. The significant effect of the increase in BAC concentration resulted in a linear decrease in drop weights for both of the dropper tips investigated. The significant effect of the dispensing angle was influenced by the dropper tip design. For the dropper tip A, the effect of the dropper tip tilt was described by the quadratic equation with a minimum, which corresponded to the dispensing angle equal to that of 48 degrees from horizontal. Below this angle, the increase in drop weights occurred due to the drop formation from the wetted external surface of the tip orifice. The linear decrease in drop weights in response to the decrease in dispensing angle was detected for the dropper tip B. The regression equations and the contour line plots obtained allowed the drop weights to be estimated for the actual combinations of both the BAC concentration and the dispensing angle. The effect of the residual volume was found to be non-significant. Based on the formula of Tate's law, the direct proportion between surface tension of a solution and the radius of the effective perimeter of a dropper tip can be used to estimate the theoretical maximal weight of drops at the dispensing angle of 90 degrees . Using the stalagmometric values of surface tension of the BAC solutions, the maximal drop weights were estimated for both of the dropper tips

  17. Delayed Frost Growth on Jumping-Drop Superhydrophobic Surfaces

    Energy Technology Data Exchange (ETDEWEB)

    Boreyko, Jonathan B [ORNL; Collier, Pat [ORNL

    2013-01-01

    Self-propelled jumping drops are continuously removed from a condensing superhydrophobic surface to enable a micrometric steady-state drop size. Here, we report that subcooled condensate on a chilled superhydrophobic surface are able to repeatedly jump off the surface before heterogeneous ice nucleation occurs. Frost still forms on the superhydrophobic surface due to ice nucleation at neighboring edge defects, which eventually spreads over the entire surface via an inter-drop frost wave. The growth of this inter-drop frost front is shown to be up to three times slower on the superhydrophobic surface compared to a control hydrophobic surface, due to the jumping-drop effect dynamically minimizing the average drop size and surface coverage of the condensate. A simple scaling model is developed to relate the success and speed of inter-drop ice bridging to the drop size distribution. While other reports of condensation frosting on superhydrophobic surfaces have focused exclusively on liquid-solid ice nucleation for isolated drops, these findings reveal that the growth of frost is an inter-drop phenomenon that is strongly coupled to the wettability and drop size distribution of the surface. A jumping-drop superhydrophobic condenser was found to be superior to a conventional dropwise condenser in two respects: preventing heterogeneous ice nucleation by continuously removing subcooled condensate, and delaying frost growth by minimizing the success of interdrop ice bridge formation.

  18. Spent Nuclear Fuel (SNF) Bounding Drop Support Calculations

    Energy Technology Data Exchange (ETDEWEB)

    CHENAULT, D.M.

    1999-11-16

    This report evaluates different drop heights, concrete and other impact media to which the transport package and/or the MCO is dropped. A prediction method is derived for estimating the resultant impact factor for determining the bounding drop case for the SNF Project.

  19. Inverse Leidenfrost Effect: Levitating Drops on Liquid Nitrogen.

    Science.gov (United States)

    Adda-Bedia, M; Kumar, S; Lechenault, F; Moulinet, S; Schillaci, M; Vella, D

    2016-05-03

    We explore the interaction between a liquid drop (initially at room temperature) and a bath of liquid nitrogen. In this scenario, heat transfer occurs through film-boiling: a nitrogen vapor layer develops that may cause the drop to levitate at the bath surface. We report the phenomenology of this inverse Leidenfrost effect, investigating the effect of the drop size and density by using an aqueous solution of a tungsten salt to vary the drop density. We find that (depending on its size and density) a drop either levitates or instantaneously sinks into the bulk nitrogen. We begin by measuring the duration of the levitation as a function of the radius R and density ρd of the liquid drop. We find that the levitation time increases roughly linearly with drop radius but depends weakly on the drop density. However, for sufficiently large drops, R ≥ Rc(ρd), the drop sinks instantaneously; levitation does not occur. This sinking of a (relatively) hot droplet induces film-boiling, releasing a stream of vapor bubbles for a well-defined length of time. We study the duration of this immersed-drop bubbling finding similar scalings (but with different prefactors) to the levitating drop case. With these observations, we study the physical factors limiting the levitation and immersed-film-boiling times, proposing a simple model that explains the scalings observed for the duration of these phenomena, as well as the boundary of (R,ρd) parameter space that separates them.

  20. Dynamics of the vapor layer below a Leidenfrost drop.

    Science.gov (United States)

    Caswell, Thomas A

    2014-07-01

    In the Leidenfrost effect a small drop of fluid is levitated, above a sufficiently hot surface, on a persistent vapor layer generated by evaporation from the drop. The vapor layer thermally insulates the drop from the surface leading to extraordinarily long drop lifetimes. The top-view shape of the levitated drops can exhibit persistent starlike vibrations. I extend recent work [Burton et al., Phys. Rev. Lett. 109, 074301 (2012)] to study the bottom surface of the drop using interference imaging. In this work I use a high-speed camera and automated image analysis to image, locate, and classify the interference fringes. From the interference fringes I reconstruct the shape and height profile of the rim where the drop is closest to the surface. I measure the drop-size dependence of the planar vibrational mode frequencies, which agree well with previous work. I observe a distinct breathing mode in the average radius of the drop, the frequency of which scales differently with drop size than the other modes. This breathing mode can be tightly coupled to a vertical motion of the drop. I further observe a qualitative difference in the structure and dynamics of the vertical profile of the rim between large and small drops.

  1. The evaporation of the charged and uncharged water drops ...

    Indian Academy of Sciences (India)

    R. Narasimhan (Krishtel eMaging) 1461 1996 Oct 15 13:05:22

    Oscillations of the drop and the change in airflow around drops are suggested to contribute to lowering of the ventilation coefficients for charged drops. Applicability of the results to a small fraction of highly charged raindrops falling through the sub-cloud layer below thunderstorm is discussed. The relaxation time required for ...

  2. Spent Nuclear Fuel (SNF) Bounding Drop Support Calculations

    International Nuclear Information System (INIS)

    CHENAULT, D.M.

    1999-01-01

    This report evaluates different drop heights, concrete and other impact media to which the transport package and/or the MCO is dropped. A prediction method is derived for estimating the resultant impact factor for determining the bounding drop case for the SNF Project

  3. Effective liquid drop description for alpha decay of atomic nuclei

    Energy Technology Data Exchange (ETDEWEB)

    Tavares, O.A.P.; Duarte, S.B. [Centro Brasileiro de Pesquisas Fisicas (CBPF), Rio de Janeiro, RJ (Brazil); Rodriguez, O.; Guzman, F. [Instituto Superior de Ciencia y Tecnologia Nuclear (ISCTN), La Habana (Cuba); Goncalves, M. [Instituto de Radioprotecao e Dosimetria (IRD), Rio de Janeiro, RJ (Brazil); Garcia, F. [Sao Paulo Univ., SP (Brazil). Inst. de Fisica

    1998-06-01

    Alpha decay half-lives are presented in the framework of an effective liquid drop model for different combination of mass transfer descriptions and inertia coefficients. Calculated half-life-values for ground-state to ground-state favoured alpha transitions are compared with available, updated experimental data. Results have shown that the present model is very suitable to treat the alpha decay process on equal foot as cluster radioactivity and cold fission processes. Better agreement with the data is found when the sub-set of even-even alpha emitters are considered in the calculation. (author) 44 refs., 5 figs., 3 tabs.; e-mail: telo at ird.gov.br

  4. Non-wetting drops at liquid interfaces: from liquid marbles to Leidenfrost drops

    Science.gov (United States)

    Wong, Clint Y. H.; Adda-Bedia, Mokhtar; Vella, Dominic

    We consider the flotation of deformable, non-wetting drops on a liquid interface. We consider the deflection of both the liquid interface and the droplet itself in response to the buoyancy forces, density difference and the various surface tensions within the system. Our results suggest new insight into a range of phenomena in which such drops occur, including Leidenfrost droplets and floating liquid marbles. In particular, we show that the floating state of liquid marbles is very sensitive to the tension of the particle-covered interface and suggest that this sensitivity may make such experiments a useful assay of the properties of these complex interfaces.

  5. Deciding between using the first or second drop of blood for the self monitoring of blood glucose.

    Science.gov (United States)

    Li, Min; Wang, Xiaoli; Shan, Zhongyan

    2014-12-01

    To explore whether the first or the second drop of blood is more suitable for the self-monitoring of blood glucose (SMBG). SMBG was employed in hospitalized patients using the first and second drop of blood. Venous blood glucose was measured meanwhile. The differences in blood glucose measurements were then compared in groups with different regions of blood glucose levels. There were 802 groups of blood glucose in 526 patients. There was no significant difference in the blood glucose levels of the first and second drop of blood and venous blood. However, after combining then dividing measurements into six groups according to blood glucose concentration, we found statistically significant differences between the blood glucose levels obtained from the first drop, second drop, and venous blood in the groups containing blood glucose values blood can be used for performing SMBG to assess real-time venous glucose. By categorizing blood glucose into different levels more accurately, we observed that there was no significant difference between the first or second drop of blood and the venous blood glucose value when blood glucose levels were maintained between 10 and 20 mmol/L. When blood glucose levels were below 10 mmol/L, the value obtained from first drop of blood was close to that from venous blood, whereas when the blood glucose level is >20 mmol/L, the blood glucose value from the second drop of blood was more accurate. Copyright © 2014 Primary Care Diabetes Europe. Published by Elsevier Ltd. All rights reserved.

  6. Comparison between solid phase microextraction (SPME) and hollow fiber liquid phase microextraction (HFLPME) for determination of extractables from post-consumer recycled PET into food simulants.

    Science.gov (United States)

    Oliveira, Éder Costa; Echegoyen, Yolanda; Cruz, Sandra Andrea; Nerin, Cristina

    2014-09-01

    Hollow fiber liquid phase microextraction (HFLPME) and solid phase microextraction (SPME) methods for pre-concentration of contaminants (toluene, benzophenone, tetracosane and chloroform) in food simulants were investigated. For HFLPME 1-heptanol, 2-octanone and dibutyl-ether were studied as extracting solvents. Analysis by gas chromatography coupled to mass spectrometry (GC-MS), flame ionization (GC-FID) and electron capture detectors (GC-ECD) were carried out. In addition, the methods were employed to evaluate the safety in use of a PET material after the recycling process (comprising washing, extrusion and solid state polymerization (SSP)) through extractability studies of the contaminants using 10% (v/v) ethanol in deionized water and 3% (w/v) acetic acid in deionized water as food simulants in different conditions: 10 days at 40°C and 2h at 70°C. The HFLPME preconcentration method provided increased sensitivity when compared to the SPME method and allowed to analyze concentration levels below 10 µg surrogate per kg food simulant. The results of the extractability studies showed considerable reductions after the extrusion and SSP processes and indicated the compliance with regulations for using recycled PET in contact with food. Copyright © 2014 Elsevier B.V. All rights reserved.

  7. Model of an Evaporating Drop Experiment

    Science.gov (United States)

    Rodriguez, Nicolas

    2017-11-01

    A computational model of an experimental procedure to measure vapor distributions surrounding sessile drops is developed to evaluate the uncertainty in the experimental results. Methanol, which is expected to have predominantly diffusive vapor transport, is chosen as a validation test for our model. The experimental process first uses a Fourier transform infrared spectrometer to measure the absorbance along lines passing through the vapor cloud. Since the measurement contains some errors, our model allows adding random noises to the computational integrated absorbance to mimic this. Then the resulting data are interpolated before passing through a computed tomography routine to generate the vapor distribution. Next, the gradients of the vapor distribution are computed along a given control volume surrounding the drop so that the diffusive flux can be evaluated as the net rate of diffusion out of the control volume. Our model of methanol evaporation shows that the accumulated errors of the whole experimental procedure affect the diffusive fluxes at different control volumes and are sensitive to how the noisy data of integrated absorbance are interpolated. This indicates the importance of investigating a variety of data fitting methods to choose which is best to present the data. Trinity University Mach Fellowship.

  8. Vlasov simulations of parallel potential drops

    Directory of Open Access Journals (Sweden)

    H. Gunell

    2013-07-01

    Full Text Available An auroral flux tube is modelled from the magnetospheric equator to the ionosphere using Vlasov simulations. Starting from an initial state, the evolution of the plasma on the flux tube is followed in time. It is found that when applying a voltage between the ends of the flux tube, about two thirds of the potential drop is concentrated in a thin double layer at approximately one Earth radius altitude. The remaining part is situated in an extended region 1–2 Earth radii above the double layer. Waves on the ion timescale develop above the double layer, and they move toward higher altitude at approximately the ion acoustic speed. These waves are seen both in the electric field and as perturbations of the ion and electron distributions, indicative of an instability. Electrons of magnetospheric origin become trapped between the magnetic mirror and the double layer during its formation. At low altitude, waves on electron timescales appear and are seen to be non-uniformly distributed in space. The temporal evolution of the potential profile and the total voltage affect the double layer altitude, which decreases with an increasing field aligned potential drop. A current–voltage relationship is found by running several simulations with different voltages over the system, and it agrees with the Knight relation reasonably well.

  9. Visualization of the impact of water drops on a hot surface: effect of drop velocity and surface inclination

    Energy Technology Data Exchange (ETDEWEB)

    Celata, Gian Piero; Mariani, Andrea; Zummo, Giuseppe [ENEA, Institute of Thermal-Fluid Dynamics, S. Maria di Galeria (Rome) (Italy); Cumo, Maurizio [Universita di Roma ' ' La Sapienza' ' , Rome (Italy)

    2006-08-15

    The behaviour of one drop impinging on a hot surface by varying the surface temperature, the drop velocity and the position of the surface (horizontal and a inclined 45 ) both at a temperature below and above the Leidenfrost temperature has been experimentally evaluated, estimating the temperature at which the drop rebounds. A large influence on the drop velocity has been evidenced. The inclination of the surface decreases the critical value of the temperature above which the surface is not rewetted. (orig.)

  10. von Kármán Vortex Street within an Impacting Drop

    KAUST Repository

    Thoraval, Marie-Jean

    2012-06-29

    The splashing of a drop impacting onto a liquid pool produces a range of different sized microdroplets. At high impact velocities, the most significant source of these droplets is a thin liquid jet emerging at the start of the impact from the neck that connects the drop to the pool. We use ultrahigh-speed video imaging in combination with high-resolution numerical simulations to show how this ejecta gives way to irregular splashing. At higher Reynolds numbers, its base becomes unstable, shedding vortex rings into the liquid from the free surface in an axisymmetric von Kármán vortex street, thus breaking the ejecta sheet as it forms.

  11. Deformed liquid marbles: Freezing drop oscillations with powders

    KAUST Repository

    Marston, Jeremy

    2012-09-01

    In this work we show that when a liquid drop impacts onto a fine-grained hydrophobic powder, the final form of the drop can be very different from the spherical form with which it impacts. In all cases, the drop rebounds due to the hydrophobic nature of the powder. However, we find that above a critical impact speed, the drop undergoes a permanent deformation to a highly non-spherical shape with a near-complete coverage of powder, which then freezes the drop oscillations during rebound. © 2012 Elsevier B.V.

  12. Air-assisted liquid–liquid microextraction by solidifying the floating organic droplets for the rapid determination of seven fungicide residues in juice samples

    Energy Technology Data Exchange (ETDEWEB)

    You, Xiangwei [Tobacco Research Institute, Chinese Academy of Agricultural Sciences, Qingdao 266101 (China); College of Science, China Agricultural University, Beijing 100193 (China); Xing, Zhuokan [College of Science, China Agricultural University, Beijing 100193 (China); Liu, Fengmao, E-mail: liufengmao@cau.edu.cn [College of Science, China Agricultural University, Beijing 100193 (China); Zhang, Xu [College of Science, China Agricultural University, Beijing 100193 (China)

    2015-05-22

    Highlights: • A novel AALLME-SFO method was firstly reported for pesticide residue analysis. • Solvent with low density and proper melting point was used as extraction solvent. • The formation of “cloudy solvent” with a syringe only. • The new method avoided the use of organic dispersive solvent. - Abstract: A novel air assisted liquid–liquid microextraction using the solidification of a floating organic droplet method (AALLME-SFO) was developed for the rapid and simple determination of seven fungicide residues in juice samples, using the gas chromatography with electron capture detector (GC-ECD). This method combines the advantages of AALLME and dispersive liquid–liquid microextraction based on the solidification of floating organic droplets (DLLME-SFO) for the first time. In this method, a low-density solvent with a melting point near room temperature was used as the extraction solvent, and the emulsion was rapidly formed by pulling in and pushing out the mixture of aqueous sample solution and extraction solvent for ten times repeatedly using a 10-mL glass syringe. After centrifugation, the extractant droplet could be easily collected from the top of the aqueous samples by solidifying it at a temperature lower than the melting point. Under the optimized conditions, good linearities with the correlation coefficients (γ) higher than 0.9959 were obtained and the limits of detection (LOD) varied between 0.02 and 0.25 μg L{sup −1}. The proposed method was applied to determine the target fungicides in juice samples and acceptable recoveries ranged from 72.6% to 114.0% with the relative standard deviations (RSDs) of 2.3–13.0% were achieved. Compared with the conventional DLLME method, the newly proposed method will neither require a highly toxic chlorinated solvent for extraction nor an organic dispersive solvent in the application process; hence, it is more environmentally friendly.

  13. Rapid characterization of trace aflatoxin B1 in groundnuts, wheat and maize by dispersive liquid-liquid microextraction followed by direct electrospray probe tandem mass spectrometry.

    Science.gov (United States)

    Satarpai, Thiphol; Siripinyanond, Atitaya; Su, Hung; Shiea, Jentaie

    2017-04-30

    Aflatoxins are poisonous and cancer-related chemical compounds commonly found in crops and plants. Aflatoxin B 1 is the most toxic compound among aflatoxins and has been classified as group 1 carcinogenic to humans, especially in liver cancer. Herein, an ambient mass spectrometric method was developed for rapid characterization of trace aflatoxin B 1 in peanuts. Direct electrospray probe tandem mass spectrometry (DEP-MS/MS) was used to detect aflatoxin B 1 in peanuts. To avoid the matrix effect, the aflatoxin B 1 in the samples was extracted and concentrated by dispersive liquid-liquid microextraction. The mass spectrometer was operated in the positive ion mode to monitor the intact molecular ion (m/z 313, MH + ) and product ion (m/z 241) of aflatoxin B 1 using multiple reaction monitoring. Since no clean-up procedure of the sample was required, the sampling step and the subsequent mass spectrometric detection of the aflatoxin B 1 was completed in less than 5 min. The limit of detection of aflatoxin B 1 is at the sub-ppb level. The results obtained by DEP-MS/MS were also validated by liquid chromatography/tandem mass spectrometry (LC/MS/MS). Recovery of aflatoxin B 1 in the sample was evaluated by analyzing spiked aflatoxin B 1 with LC/MS/MS to be 85% and DEP-MS/MS to be 84%. DEP-MS/MS combined with a simple dispersive liquid-liquid microextraction procedure was successfully used for the quantitative analysis of AFB 1 in nut samples. Due to its high efficiency, it is promising in providing important toxicological information for food safety in the real world. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

  14. Simultaneous determination of several phytohormones in natural coconut juice by hollow fiber-based liquid-liquid-liquid microextraction-high performance liquid chromatography.

    Science.gov (United States)

    Wu, Yunli; Hu, Bin

    2009-11-06

    A simple, selective, sensitive and inexpensive method of hollow fiber-based liquid-liquid-liquid microextraction (HF-LLLME) combined with high performance liquid chromatography (HPLC)-ultraviolet (UV) detection was developed for the determination of four acidic phytohormones (salicylic acid (SA), indole-3-acetic acid (IAA), (+/-) abscisic acid (ABA) and (+/-) jasmonic acid (JA)) in natural coconut juice. To the best of our knowledge, this is the first report on the use of liquid phase microextraction (LPME) as a sample pretreatment technique for the simultaneous analysis of several phytohormones. Using phenetole to fill the pores of hollow fiber as the organic phase, 0.1molL(-1) NaOH solution in the lumen of hollow fiber as the acceptor phase and 1molL(-1) HCl as the donor phase, a simultaneous preconcentration of four target phytohormones was realized. The acceptor phase was finally withdrawn into the microsyringe and directly injected into HPLC for the separation and quantification of the target phytohormones. The factors affecting the extraction efficiency of four phytohormones by HF-LLLME were optimized with orthogonal design experiment, and the data was analyzed by Statistical Product and Service Solutions (SPSS) software. Under the optimized conditions, the enrichment factors for SA, IAA, ABA and JA were 243, 215, 52 and 48, with the detection limits (S/N=3) of 4.6, 1.3, 0.9ngmL(-1) and 8.8 microg mL(-1), respectively. The relative standard deviations (RSDs, n=7) were 7.9, 4.9, 6.8% at 50ngmL(-1) level for SA, IAA, ABA and 8.4% at 500 microg mL(-1) for JA, respectively. To evaluate the accuracy of the method, the developed method was applied for the simultaneous analysis of several phytohormones in five natural coconut juice samples, and the recoveries for the spiked samples were in the range of 88.3-119.1%.

  15. In situ metathesis ionic liquid formation dispersive liquid-liquid microextraction for copper determination in water samples by electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Stanisz, Ewa; Zgoła-Grześkowiak, Agnieszka

    2013-10-15

    In situ synthesis of ionic liquid extractant for dispersive liquid-liquid microextraction (in situ IL DLLME) combined with electrothermal atomic absorption spectrometry (ET AAS) for determination of copper in water samples was developed. Analytical signals were obtained without the back-extraction of copper from the IL phase prior to its determination by AAS. Some essential parameters of the microextraction and detection techniques such as the pH of sample solution, volume of components for in situ synthesis, matrix interferences and main parameters of graphite furnace atomizer have been studied. Under optimal conditions, high extraction efficiency for copper was achieved for the extraction of 0.7 µg L(-1) in 10.0 mL of sample solution employing 8 μL of 1-hexyl-3-methylimidazolium bis[(trifluoromethyl)sulfonyl]imide (HmimNTf2) as the extraction solvent. The detection limit was found as 0.004 µg L(-1) with an enrichment factor of 200. The relative standard deviation (RSD) for seven replicate measurements of 0.7 µg L(-1) in sample solution was 4%. The accuracy of the proposed method was evaluated by analysis of the Certified Reference Materials: NIST SRM 2709 (San Joaquin Soil), NBS SRM 2704 (Buffalo River Sediment), NRCC DOLT-2 (Dogfish Liver) and NIST SRM 1643e (Trace Element in Water). The measured copper contents in the reference materials were in satisfactory agreement with the certified values. The method was successfully applied to analysis of the tap, lake and mineral water samples. © 2013 Elsevier B.V. All rights reserved.

  16. Air-assisted liquid–liquid microextraction by solidifying the floating organic droplets for the rapid determination of seven fungicide residues in juice samples

    International Nuclear Information System (INIS)

    You, Xiangwei; Xing, Zhuokan; Liu, Fengmao; Zhang, Xu

    2015-01-01

    Highlights: • A novel AALLME-SFO method was firstly reported for pesticide residue analysis. • Solvent with low density and proper melting point was used as extraction solvent. • The formation of “cloudy solvent” with a syringe only. • The new method avoided the use of organic dispersive solvent. - Abstract: A novel air assisted liquid–liquid microextraction using the solidification of a floating organic droplet method (AALLME-SFO) was developed for the rapid and simple determination of seven fungicide residues in juice samples, using the gas chromatography with electron capture detector (GC-ECD). This method combines the advantages of AALLME and dispersive liquid–liquid microextraction based on the solidification of floating organic droplets (DLLME-SFO) for the first time. In this method, a low-density solvent with a melting point near room temperature was used as the extraction solvent, and the emulsion was rapidly formed by pulling in and pushing out the mixture of aqueous sample solution and extraction solvent for ten times repeatedly using a 10-mL glass syringe. After centrifugation, the extractant droplet could be easily collected from the top of the aqueous samples by solidifying it at a temperature lower than the melting point. Under the optimized conditions, good linearities with the correlation coefficients (γ) higher than 0.9959 were obtained and the limits of detection (LOD) varied between 0.02 and 0.25 μg L −1 . The proposed method was applied to determine the target fungicides in juice samples and acceptable recoveries ranged from 72.6% to 114.0% with the relative standard deviations (RSDs) of 2.3–13.0% were achieved. Compared with the conventional DLLME method, the newly proposed method will neither require a highly toxic chlorinated solvent for extraction nor an organic dispersive solvent in the application process; hence, it is more environmentally friendly

  17. Nanometer-sized ceria-coated silica-iron oxide for the reagentless microextraction/preconcentration of heavy metals in environmental and biological samples followed by slurry introduction to ICP-OES.

    Science.gov (United States)

    Dados, A; Paparizou, E; Eleftheriou, P; Papastephanou, C; Stalikas, C D

    2014-04-01

    A slurry suspension sampling technique is developed and optimized for the rapid microextraction of heavy metals and analysis using nanometer-sized ceria-coated silica-iron oxide particles and inductively coupled plasma optical emission spectrometry (ICP-OES). Magnetic-silica material is synthesized by a co-precipitation and sol-gel method followed by ceria coating through a precipitation. The large particles are removed using a sedimentation-fractionation procedure and a magnetic homogeneous colloidal suspension of ceria-modified iron oxide-silica is produced for microextraction. The nanometer-sized particles are separated from the sample solution magnetically and analyzed with ICP-OES using a slurry suspension sampling approach. The ceria-modified iron oxide-silica does not contain any organic matter and this probably justifies the absence of matrix effect on plasma atomization capacity, when increased concentrations of slurries are aspirated. The As, Be, Mo, Cr, Cu, Pb, Hg, Sb, Se and V can be preconcentrated by the proposed method at pH 6.0 while Mn, Cd, Co and Ni require a pH ≥ 8.0. Satisfactory values are obtained for the relative standard deviations (2-6%), recoveries (88-102%), enrichment factors (14-19) and regression correlation coefficients as well as detectability, at sub-μg L(-1) levels. The applicability of magnetic ceria for the microextraction of metal ions in combination with the slurry introduction technique using ICP is substantiated by the analysis of environmental water and urine samples. Copyright © 2013 Elsevier B.V. All rights reserved.

  18. Optical Detection and Magnetic Manipulation of Drops in Microfluidic Devices

    Science.gov (United States)

    Kerbage, Charles

    2005-03-01

    We demonstrate an integrated magneto-optic microfluidic device for drop detection and sorting. Optical detection of water drops formed in a continuous oil phase flow is performed using optical fibers which are integrated into the channels of the PDMS (Polydimethylsiloxane) based microfluidic device. The size and the velocity of the drops can be determined by measuring the transmission intensity as a function of time. We also show that such a device can be used to detect fluorescent materials introduced in the drop itself. Moreover, introducing nano-scale magnetic particles into the water drops allows for drop sorting by means of a magnetic field gradient. This magnetic field is generated through thin film permalloy integrated into the device itself and tuned by an external coil. We show that the sorting depends on the magnetic field gradient, material composite and volume fraction of the magnetic material in the drops.

  19. Jumps, somersaults, and symmetry breaking in Leidenfrost drops

    Science.gov (United States)

    Chen, Simeng; Bertola, Volfango

    2016-08-01

    When a droplet of water impacts a heated surface, the drop may be observed to bounce. Recently is has been found that small quantities (˜100 ppm) of polymer additives such as polyethylene oxide can significantly increase the maximum bouncing height of drops. This effect has been explained in terms of the reduction of energy dissipation caused by polymer additives during the drop retraction and rebound, resulting in higher mechanical energy available for bouncing. Here we demonstrate, by comparing three types of fluids (Newtonian, shear-thinning, and viscoelastic), that the total kinetic energy carried by low-viscosity Newtonian drops during retraction is partly transformed into rotational kinetic energy rather than dissipated when compared with high-viscosity or non-Newtonian drops. We also show that non-Newtonian effects play little role in the energy distribution during drop impact, while the main effect is due to the symmetry break observed during the retraction of low-viscosity drops.

  20. IMPACT ANALYSIS OF SPENT FUEL DRY CASKS UNDER ACCIDENTAL DROP SCENARIOS

    International Nuclear Information System (INIS)

    BRAVERMAN, J.I.; MORANTE, R.J.; XU, J.; HOFMAYER, C.H.; SHAUKAT, S.K.

    2003-01-01

    A series of analyses were performed to assess the structural response of spent nuclear fuel dry casks subjected to various handling and on-site transfer events. The results of these analyses are being used by the Nuclear Regulatory Commission (NRC) to perform a probabilistic risk assessment (PRA). Although the PRA study is being performed for a specific nuclear plant, the PRA study is also intended to provide a framework for a general methodology that could also be applied to other dry cask systems at other nuclear plants. The dry cask system consists of a transfer cask, used for handling and moving the multi-purpose canister OLIIpC that contains the fuel, and a storage cask, used to store the MPC and fuel on a concrete pad at the site. This paper describes the analyses of the casks for two loading events. The first loading consists of dropping the transfer cask while it is lowered by a crane to a concrete floor at ground elevation. The second loading consists of dropping the storage cask while it is being transferred to the concrete storage pad outdoors. Three dimensional finite element models of the transfer cask and storage cask, containing the MPC and fuel, were utilized to perform the drop analyses. These models were combined with finite element models of the target structures being impacted. The transfer cask drop analyses considered various drop heights for the cask impacting the reinforced concrete floor at ground level. The finite element model of the target included a section of the concrete floor and concrete wall supporting the floor. The storage cask drop analyses evaluated a 30.5 cm (12 in.) drop of the cask impacting three different surfaces: reinforced concrete, asphalt, and gravel

  1. Finite size effects on textured surfaces: recovering contact angles from vagarious drop edges.

    Science.gov (United States)

    Gauthier, Anaïs; Rivetti, Marco; Teisseire, Jérémie; Barthel, Etienne

    2014-02-18

    A clue to understand wetting hysteresis on superhydrophobic surfaces is the relation between receding contact angle and surface textures. When the surface textures are large, there is a significant distribution of local contact angles around the drop. As seen from the cross section, the apparent contact angle oscillates as the triple line recedes. Our experiments demonstrate that the origin of these oscillations is a finite size effect. Combining side and bottom views of the drop, we take into account the 3D conformation of the surface near the edge to evaluate an intrinsic contact angle from the oscillations of the apparent contact angle. We find that for drops receding on axisymmetric textures the intrinsic receding contact angle is the minimum value of the oscillation while for a square lattice it is the maximum.

  2. Drop Pinch-Off for Discrete Flows from a Capillary

    Directory of Open Access Journals (Sweden)

    Wilson M.C.T.

    2013-07-01

    Full Text Available The problem of drop formation and pinch-off from a capillary tube under the influence of gravity has been extensively studied when the internal capillary pressure gradient is constant. This ensures a continuous time independent flow field inside the capillary tube typically of the Poiseuille flow type. Characteristic drop ejection behaviour includes: periodic drop ejection, drop ejection with associated satellite production, complex dripping, chaotic behaviour and jetting. It is well known that this characteristic behaviour is governed by the Weber (We and Ohnesorge (Oh numbers (for a given Bond number and may be delineated in a We verses Oh operability diagram. An in-depth physical understanding of drop ejection is also of great importance to industry where the tight control of drop size and ejection velocity are of critical importance in industrial processes such as sealants used in electronics assembly and inkjet printing. However, the use of such a continuous flow approach for drop ejection in industry is often impractical since such flows cannot be operator controlled. For this reason it is important to investigate so-called discrete pipe flows where the flow can be turned on and off at will. This means the flow inside the pipe is now time-dependent being controlled in a step-wise fashion. As a first stage in the investigation of drop pinch-off behaviour in discrete pipe flows this paper will study the critical pinch-off time required for drop ejection starting from a pendant drop. This is the discrete amount of time the pipe flow is turned on for in order for a drop to be ejected from the capillary. A Newtonian incompressible free-surface CFD flow code developed at the University of Leeds is used to investigate the critical pinch-off time for a range of internal pipe velocities (the central flow maximum in Poiseuille flow. It is found that the time required for drop ejection to occur decreases exponentially with internal pipe velocity

  3. Crack formation and prevention in colloidal drops

    Science.gov (United States)

    Kim, Jin Young; Cho, Kun; Ryu, Seul-A.; Kim, So Youn; Weon, Byung Mook

    2015-08-01

    Crack formation is a frequent result of residual stress release from colloidal films made by the evaporation of colloidal droplets containing nanoparticles. Crack prevention is a significant task in industrial applications such as painting and inkjet printing with colloidal nanoparticles. Here, we illustrate how colloidal drops evaporate and how crack generation is dependent on the particle size and initial volume fraction, through direct visualization of the individual colloids with confocal laser microscopy. To prevent crack formation, we suggest use of a versatile method to control the colloid-polymer interactions by mixing a nonadsorbing polymer with the colloidal suspension, which is known to drive gelation of the particles with short-range attraction. Gelation-driven crack prevention is a feasible and simple method to obtain crack-free, uniform coatings through drying-mediated assembly of colloidal nanoparticles.

  4. Drop Impact on a Solid Surface

    KAUST Repository

    Josserand, C.

    2015-09-22

    © Copyright 2016 by Annual Reviews. All rights reserved. A drop hitting a solid surface can deposit, bounce, or splash. Splashing arises from the breakup of a fine liquid sheet that is ejected radially along the substrate. Bouncing and deposition depend crucially on the wetting properties of the substrate. In this review, we focus on recent experimental and theoretical studies, which aim at unraveling the underlying physics, characterized by the delicate interplay of not only liquid inertia, viscosity, and surface tension, but also the surrounding gas. The gas cushions the initial contact; it is entrapped in a central microbubble on the substrate; and it promotes the so-called corona splash, by lifting the lamella away from the solid. Particular attention is paid to the influence of surface roughness, natural or engineered to enhance repellency, relevant in many applications.

  5. Drop Impact on to Moving Liquid Pools

    Science.gov (United States)

    Muñoz-Sánchez, Beatriz Natividad; Castrejón-Pita, José Rafael; Castrejón-Pita, Alfonso Arturo; Hutchings, Ian M.

    2014-11-01

    The deposition of droplets on to moving liquid substrates is an omnipresent situation both in nature and industry. A diverse spectrum of phenomena emerges from this simple process. In this work we present a parametric experimental study that discerns the dynamics of the impact in terms of the physical properties of the fluid and the relative velocity between the impacting drop and the moving liquid pool. The behaviour ranges from smooth coalescence (characterized by little mixing) to violent splashing (generation of multiple satellite droplets and interfacial vorticity). In addition, transitional regimes such as bouncing and surfing are also found. We classify the system dynamics and show a parametric diagram for the conditions of each regime. This work was supported by the EPSRC (Grant EP/H018913/1), the Royal Society, Becas Santander Universidades and the International Relationships Office of the University of Extremadura.

  6. Shape oscillations of a viscoelastic drop

    International Nuclear Information System (INIS)

    Khismatullin, Damir B.; Nadim, Ali

    2001-01-01

    Small-amplitude axisymmetric shape deformations of a viscoelastic liquid drop in microgravity are theoretically analyzed. Using the Jeffreys constitutive equation for linear viscoelasticity, the characteristic equation for the frequency and decay factor of the shape oscillations is derived. Asymptotic analysis of this equation is performed in the low- and high-viscosity limits and for the cases of small, moderate, and large elasticities. Elastic effects are shown to give rise to a type of shape oscillation that does not depend on the surface tension. The existence of such oscillations is confirmed by numerical solution of the characteristic equation in various regimes. A method for determining the viscoelastic properties of highly viscous liquids based upon experimental measurements of the frequency and damping rate of such shape oscillations is suggested

  7. Horizontal Drop of 21- PWR Waste Package

    International Nuclear Information System (INIS)

    A.K. Scheider

    2001-01-01

    The objective of this calculation is to determine the structural response of the waste package (WP) dropped horizontally from a specified height. The WP used for that purpose is the 21-Pressurized Water Reactor (PWR) WP. The scope of this document is limited to reporting the calculation results in terms of stress intensities. The information provided by the sketches (Attachment I) is that of the potential design of the type of WP considered in this calculation, and all obtained results are valid for that design only. This calculation is associated with the WP design and was performed by the Waste Package Design group in accordance with the ''Technical Work Plan for: Waste Package Design Description for LA'' (Ref. 16). AP-3.12Q, ''Calculations'' (Ref. 11) is used to perform the calculation and develop the document. The sketches attached to this calculation provide the potential dimensions and materials for the 21-PWR WP design

  8. Performance of PrekotAC Filter Aids on Pressure Drop across Two Different Filter Media

    Directory of Open Access Journals (Sweden)

    Hajar S.

    2017-01-01

    Full Text Available A study on the performance of formulated PrekotAC filter aids on pressure drop across two different types of filter media, i.e polytetrafluoroethylene (PTFE and polyimide (P84 was carried out in a laboratory scale fabric filtration system. Filter aids is applied in order to prolong the lifespan of the fabric filter by reducing the pressure drop across a filter cake. PrekotAC which is a combination of 90%wt activated carbon and 10%wt PreKotTM was tested under various material loadings of 0.2, 0.4, and 0.6 mg/mm2 at a constant filtration velocity of 5 m/min across its cake and filter media. The results showed that PrekotAC presents a lower pressure drop across the P84 compared to PTFE filter media under various material loadings. This is because of its different characteristics that effect the porosity of the filter media and allow a higher volumetric airflow passing through, resulting in lower pressure drop compared to PTFE filter media. In addition, the diversity in terms of particle size distribution of the formulated PrekotAC that increase its permeability property helps to reduce the pressure drop across the media and its filter cake. Thus, PrekotAC has a promising characteristic as a two in one filter aids, a pre-coating and adsorbent material for fabric filtration system.

  9. Spontaneous jumping, bouncing and trampolining of hydrogel drops on a heated plate.

    Science.gov (United States)

    Pham, Jonathan T; Paven, Maxime; Wooh, Sanghyuk; Kajiya, Tadashi; Butt, Hans-Jürgen; Vollmer, Doris

    2017-10-13

    The contact between liquid drops and hot solid surfaces is of practical importance for industrial processes, such as thermal spraying and spray cooling. The contact and bouncing of solid spheres is also an important event encountered in ball milling, powder processing, and everyday activities, such as ball sports. Using high speed video microscopy, we demonstrate that hydrogel drops, initially at rest on a surface, spontaneously jump upon rapid heating and continue to bounce with increasing amplitudes. Jumping is governed by the surface wettability, surface temperature, hydrogel elasticity, and adhesion. A combination of low-adhesion impact behavior and fast water vapor formation supports continuous bouncing and trampolining. Our results illustrate how the interplay between solid and liquid characteristics of hydrogels results in intriguing dynamics, as reflected by spontaneous jumping, bouncing, trampolining, and extremely short contact times.Drops of liquid on a hot surface can exhibit fascinating behaviour such as the Leidenfrost effect in which drops hover on a vapour layer. Here Pham et al. show that when hydrogel drops are placed on a rapidly heated plate they bounce to increasing heights even if they were initially at rest.

  10. Investigation of the quality of stored red blood cells after simulated air drop in the maritime environment.

    Science.gov (United States)

    Meli, Athinoula; Hancock, Vicky; Doughty, Heidi; Smedley, Steve; Cardigan, Rebecca; Wiltshire, Michael

    2018-02-01

    Maritime medical capability may be compromised by blood resupply. Air-dropped red blood cells (RBCs) is a possible mitigation factor. This study set out to evaluate RBC storage variables after a simulated parachute air drop into the sea, as limited data exist. The air load construction for the air drop of blood was subject to static drop assessment to simulate a worst-case parachute drop scenario. One control and two test Golden Hour shipping containers were each packaged with 10 RBC units. The control box was not dropped; Test Boxes 1 and 2 were further reinforced with waterproof boxes and underwent a simulated air drop on Day 7 or Day 8 postdonation, respectively. One day after the drop and once a week thereafter until Day 43 of storage, RBCs from each box were sampled and tested for full blood counts, hemolysis, adenosine triphosphate, 2,3-diphosphoglycerate, pH, extracellular potassium, glucose, lactate, deformability, and RBC microvesicles. The packaging configuration completed the air drop with no water ingress or physical damage. All units met UK specifications for volume, hemoglobin, and hemolysis. There were no significant differences for any of the variables studied between RBCs in the control box compared to RBCs in Test Boxes 1 and 2 combined over storage. The test proved that the packaging solution and the impact of a maritime air drop as performed in this study, on Day 7 or Day 8 postdonation, did not affect the in vitro quality of RBCs in SAGM over storage for 35 days. © 2017 AABB.

  11. Marangoni Flow Induced Evaporation Enhancement on Binary Sessile Drops.

    Science.gov (United States)

    Chen, Pin; Harmand, Souad; Ouenzerfi, Safouene; Schiffler, Jesse

    2017-06-15

    The evaporation processes of pure water, pure 1-butanol, and 5% 1-butanol aqueous solution drops on heated hydrophobic substrates are investigated to determine the effect of temperature on the drop evaporation behavior. The evolution of the parameters (contact angle, diameter, and volume) during evaporation measured using a drop shape analyzer and the infrared thermal mapping of the drop surface recorded by an infrared camera were used in investigating the evaporation process. The pure 1-butanol drop does not show any thermal instability at different substrate temperatures, while the convection cells created by the thermal Marangoni effect appear on the surface of the pure water drop from 50 °C. Because 1-butanol and water have different surface tensions, the infrared video of the 5% 1-butanol aqueous solution drop shows that the convection cells are generated by the solutal Marangoni effect at any substrate temperature. Furthermore, when the substrate temperature exceeds 50 °C, coexistence of the thermal and solutal Marangoni flows is observed. By analyzing the relation between the ratio of the evaporation rate of pure water and 1-butanol aqueous solution drops and the Marangoni number, a series of empirical equations for predicting the evaporation rates of pure water and 1-butanol aqueous solution drops at the initial time as well as the equations for the evaporation rate of 1-butanol aqueous solution drop before the depletion of alcohol are derived. The results of these equations correspond fairly well to the experimental data.

  12. Drop Test Results of CRDM under Seismic Loads

    International Nuclear Information System (INIS)

    Choi, Myoung-Hwan; Cho, Yeong-Garp; Kim, Gyeong-Ho; Sun, Jong-Oh; Huh, Hyung

    2016-01-01

    This paper describes the test results to demonstrate the drop performance of CRDM under seismic loads. The top-mounted CRDM driven by the stepping motor for Jordan Research and Training Reactor (JRTR) has been developed in KAERI. The CRDM for JRTR has been optimized by the design improvement based on that of the HANARO. It is necessary to verify the drop performance under seismic loads such as operating basis earthquake (OBE) and safe shutdown earthquake (SSE). Especially, the CAR drop times are important data for the safety analysis. confirm the drop performance under seismic loads. The delay of drop time at Rig no. 2 due to seismic loads is greater than that at Rig no. 3. The total pure drop times under seismic loads are estimated as 1.169 and 1.855, respectively

  13. The Influence of Concentrace Mineral Drops on Performance Broiler

    Directory of Open Access Journals (Sweden)

    Sigit Mugiyono

    1999-05-01

    Full Text Available A research has been conducted in Experimental Farm Faculty of Animal Husbandry Unsoed from July 1 st until August 15 th, 1996. The purpose want to study the influence of CMD supplementation in drinking water consists of M0 = control; M1 = 0.5 drops/1000 cc, M2 = 1 drops/1000 cc; M3 = 1.5 drops/1000 cc and M4 = 2 drops/1000cc. The performance observed were growth, body weight, feed consumption, feed conversion, drinking water consumption; and income over feed and mineral cost (IOFMC. The research involved 100 broiler chickens divided that CMD supplementation until 2 drops/1000cc did not significantly affect on the performance of broiler chickens except in income over feed and mineral cost (P<0.05. (Animal Production 1(2: 56-62 (1999 Key Words: broiler, concentrace mineral drops, performance.

  14. A study of fungi on droppings of certain birds

    Directory of Open Access Journals (Sweden)

    C. S. Singh

    2014-08-01

    Full Text Available Droppings of fowl, owl, parrot, pigeon and sparrow were asepticaly collected in sterilized bottles from different places at Gorakhpur, 54 fungi were isolated. The number of fungi was more in the pigeon showing considerable decrease in the fowl and the sparrow. In the parrot and the owl, however. the fungi were egual in number. The number of Phycomycetes was almost the same on droppings of all birds, from parrot only one species could be isolated. A larger number of Ascomyteces was recorded from fowl, less from pigeon and owl and the least (two each on sparrow and parrot droppings. The Basidiomycetes, represented by two species only, were recorded on owl and pigeon droppings. Pigeon droppings yielded the largest number of Deuteromycetes. They were egual in numbers on owl and parrot while on fowl and sparrow their number was comparatively less. Mycelia sterilia, though poor in their numbers, were recorded on all the bird droppings excepting owl.

  15. Drop Impact on Textile Material: Effect of Fabric Properties

    Directory of Open Access Journals (Sweden)

    Romdhani Zouhaier

    2014-09-01

    Full Text Available This paper presents an experimental study of impact of water drop on a surface in a spreading regime with no splashing. Three surfaces were studied: virgin glass, coating film and woven cotton fabric at different construction parameters. All experiments were carried out using water drop with the same free fall high. Digidrop with high-resolution camera is used to measure the different parameters characterising this phenomenon. Results show an important effect of the height of the free fall on the drop profile and the spreading behaviour. An important drop deformation at the surface impact was observed. Then, fabric construction as the weft count deeply affects the drop impact. For plain weave, an increase of weft count causes a decrease in penetration and increase in the spreading rate. The same result was obtained for coated fabric. Therefore, the impact energy was modified and the drop shape was affected, which directly influenced the spreading rate.

  16. Evaporation of a sessile water drop and a drop of aqueous salt solution.

    Science.gov (United States)

    Misyura, S Y

    2017-11-07

    The influence of various factors on the evaporation of drops of water and aqueous salt solution has been experimentally studied. Typically, in the studies of drop evaporation, only the diffusive vapor transfer, radiation and the molecular heat conduction are taken into account. However, vapor-gas convection plays an important role at droplet evaporation. In the absence of droplet boiling, the influence of gas convection turns out to be the prevailing factor. At nucleate boiling, a prevailing role is played by bubbles generation and vapor jet discharge at a bubble collapse. The gas convection behavior for water and aqueous salt solution is substantially different. With a growth of salt concentration over time, the influence of the convective component first increases, reaches an extremum and then significantly decreases. At nucleate boiling in a salt solution it is incorrect to simulate the droplet evaporation and the heat transfer in quasi-stationary approximation. The evaporation at nucleate boiling in a liquid drop is divided into several characteristic time intervals. Each of these intervals is characterized by a noticeable change in both the evaporation rate and the convection role.

  17. Drop-out from a psychodynamic group psychotherapy outpatient unit.

    Science.gov (United States)

    Jensen, Hans Henrik; Mortensen, Erik Lykke; Lotz, Martin

    2014-11-01

    BACKGROUND. Drop-out from psychotherapy is common and represents a considerable problem in clinical practice and research. Aim. To explore pre-treatment predictors of early and late drop-out from psychodynamic group therapy in a public outpatient unit for non-psychotic disorders in Denmark. Methods. Naturalistic design including 329 patients, the majority with mood, neurotic and personality disorders referred to 39-session group therapy. Predictors were socio-demographic and clinical variables, self-reported symptoms (Symptom Check List-90-Revised) and personality style (Millon Clinical Multiaxial Inventory-II). Drop-out was classified into early and late premature termination excluding patients who dropped out for external reasons. Results. Drop-out comprised 20.6% (68 patients) of the sample. Logistic regression revealed social functioning, vocational training, alcohol problems and antisocial behavior to be related to drop-out. However, early drop-outs had prominent agoraphobic symptoms, lower interpersonal sensitivity and compulsive personality features, and late drop-outs cognitive and somatic anxiety symptoms and antisocial personality features. Clinical and psychological variables accounted for the major part of variance in predictions of drop-out, which ranged from 15.6% to 19.5% (Nagelkerke Pseudo R-Square). Conclusion. Social functioning was consistently associated with drop-out, but personality characteristics and anxiety symptoms differentiated between early and late drop-out. Failure to discriminate between stages of premature termination may explain some of the inconsistencies in the drop-out literature. Clinical implications. Before selection of patients to time-limited psychodynamic groups, self-reported symptoms should be thoroughly considered. Patients with agoraphobic symptoms should be offered alternative treatment. Awareness of and motivation to work with interpersonal issues may be essential for compliance with group therapy.

  18. Isolation of Indonesian Cananga oil by instantaneous controlled pressure drop

    OpenAIRE

    2008-01-01

    The isolation of cananga oil by a new process, Instantaneous Controlled Pressure Drop (DIC), was investigated. This process consists in heating the dry cananga (Cananga odorata Hook. fil. et Thomson,forma macrophylla) flowers for a short time period by steam, followed by an abrupt pressure drop into a vacuum (about 5 kPa). This pressure drop provokes auto-vaporization of the volatile compounds, puffing of flowers, breaking of cell walls and cooling. The effect of the process parameters, namel...

  19. Drop impact and rebound dynamics on an inclined superhydrophobic surface.

    Science.gov (United States)

    Yeong, Yong Han; Burton, James; Loth, Eric; Bayer, Ilker S

    2014-10-14

    Due to its potential in water-repelling applications, the impact and rebound dynamics of a water drop impinging perpendicular to a horizontal superhydrophobic surface have undergone extensive study. However, drops tend to strike a surface at an angle in applications. In such cases, the physics governing the effects of oblique impact are not well studied or understood. Therefore, the objective of this study was to conduct an experiment to investigate the impact and rebound dynamics of a drop at various liquid viscosities, in an isothermal environment, and on a nanocomposite superhydrophobic surface at normal and oblique impact conditions (tilted at 15°, 30°, 45°, and 60°). This study considered drops falling from various heights to create normal impact Weber numbers ranging from 6 to 110. In addition, drop viscosity was varied by decreasing the temperature for water drops and by utilizing water-glycerol mixtures, which have similar surface tension to water but higher viscosities. Results revealed that oblique and normal drop impact behaved similarly (in terms of maximum drop spread as well as rebound dynamics) at low normal Weber numbers. However, at higher Weber numbers, normal and oblique impact results diverged in terms of maximum spread, which could be related to asymmetry and more complex outcomes. These asymmetry effects became more pronounced as the inclination angle increased, to the point where they dominated the drop impact and rebound characteristics when the surface was inclined at 60°. The drop rebound characteristics on inclined surfaces could be classified into eight different outcomes driven primarily by normal Weber number and drop Ohnesorge numbers. However, it was found that these outcomes were also a function of the receding contact angle, whereby reduced receding angles yielded tail-like structures. Nevertheless, the contact times of the drops with the coating were found to be generally independent of surface inclination.

  20. Self-excited hydrothermal waves in evaporating sessile drops

    OpenAIRE

    Sefiane K.; Moffat J.R.; Matar O.K.; Craster R.V.

    2008-01-01

    Pattern formation driven by the spontaneous evaporation of sessile drops of methanol, ethanol, and FC-72 using infrared thermography is observed and, in certain cases, interpreted in terms of hydrothermal waves. Both methanol and ethanol drops exhibit thermal wave trains, whose wave number depends strongly on the liquid volatililty and substrate thermal conductivity. The FC- 72 drops develop cellular structures whose size is proportional to the local thickness. Prior to this work, hydrotherma...

  1. Studying the field induced breakup of acoustically levitated drops

    Science.gov (United States)

    Warschat, C.; Riedel, J.

    2017-10-01

    Coulomb fission of charged droplets (The terms drop and droplet are often used synonymous. Throughout this manuscript, to avoid confusion, the terms drop and droplet will be used for liquid spheres with radii in the millimeter range and the micrometer range, respectively. In our experiments, the first correspond to the parent drop while the latter describes the ejected progeny droplets.) is a well-studied natural phenomenon. Controlled droplet fission is already successfully employed in several technological applications. Still, since the occurring surface rupture relies on the exact understanding and description of the liquid gas boundary, some details are still under debate. Most empirical systematic studies observe falling micrometer droplets passing through the electric field inside a plate capacitor. This approach, although easily applicable and reliable, limits the experimental degrees of freedom regarding the observable time and the maximum size of the drops and can only be performed in consecutive individual observations of different subsequent drops. Here we present a novel setup to study the field induced breakup of acoustically levitated drops. The design does not bear any restrictions towards the temporal window of observation, and allows handling of drops of a tunable radius ranging from 10 μm to several millimeters and a real-time monitoring of one single drop. Our comprehensive study includes a time resolved visual inspection, laser shadowgraphy, laser induced fluorescence imaging, and ambient mass spectrometric interrogation of the nascent Taylor cone. The results shown for a millimeter sized drop, previously inaccessible for Coulomb fission experiments, are mostly comparable with previous results for smaller drops. The major difference is the time scale and the threshold potential of the drop rupture. Both values, however, resemble theoretically extrapolations to the larger radius. The technique allows for a systematic study of breakup behavior of

  2. Confined thermocapillary motion of a three-dimensional deformable drop

    Science.gov (United States)

    Brady, P. T.; Herrmann, M.; Lopez, J. M.

    2011-02-01

    In this paper, simulations are performed of the thermocapillary motion of three-dimensional and axisymmetric drops in a confined apparatus. The refined level-set grid method is used to track the interface and resolve very small deformations. We compare our results to theoretically predicted thermocapillary migration velocities of drops and to experimentally measured migration velocities in microgravity experiments. The motivation of the present work is to address four important questions surrounding thermocapillary migration. These are as follows. (1) What is the impact of initial conditions on both the initial transient and steady state drop behavior? (2) What is the impact of the domain geometry on drop behavior? (3) Do drops deform for intermediate Marangoni numbers and are those deformations axisymmetric? (4) Can the assumption of constant temperature fluid properties be used when simulating physical experiments? To answer the first question, we explore the parameter space of initial drop temperature distribution and drop holding time. We find that in lower Marangoni number regimes, the drop rapidly settles to a quasisteady state. For larger Marangoni numbers, the initial conditions dominate the drop behavior. To address the second and third questions, we look at the spatial distribution of tangential temperature gradients on the surface of the drop as well as drop deformations and migration velocities. The domain geometry induces nonaxisymmetric deformations and temperature distributions. The results of several axisymmetric runs with realistic physical properties are examined to answer the fourth question. It is found that the variation of material properties influences the drop migration behavior in a nontrivial way.

  3. Reducing Variability in Stress Drop with Root-Mean Acceleration

    Science.gov (United States)

    Crempien, J.; Archuleta, R. J.

    2012-12-01

    Stress drop is a fundamental property of the earthquake source. For a given tectonic region stress drop is assumed to be constant allowing for the scaling of earthquake spectra. However, the variability of the stress drop, either for worldwide catalogs or regional catalogs, is quite large. The variability around the median value is on the order of 1.5 in log10 units. One question that continues to pervade the analysis of stress drop is whether this variability is an inherent characteristic of the Earth or is an artifact of the determination of stress drop via the use of the spectral analysis. It is simple to see that the stress drop determined by seismic moment times corner frequency cubed that errors in the corner frequency will strongly influence the variability in the stress drop. To avoid this strong dependence on corner frequency cubed, we have examined the determination of stress drop based on the approach proposed by Hanks (1979), namely using the root-mean-square acceleration. The stress drop determined using rms acceleration may be advantageous because the stress drop is only affected by the square root of the corner frequency. To test this approach we have determined stress drops for the 2000 Tottori earthquake and its aftershocks. We use both the classic method of fitting to a spectrum as well as using rms acceleration. For a preliminary analysis of eight aftershocks and the mainshock we find that the variability in stress drop is reduced by about a factor of two. This approach needs more careful analysis of more events, which will be shown at the meeting.

  4. Determination of parathion in biological fluids by means of direct Solid Phase Microextraction.

    OpenAIRE

    Gallardo, Eugenia; Barroso, Mário; Margalho, C.; Cruz, Angelines; Vieira, Duarte Nuno; López-Rivadulla, Manuel

    2010-01-01

    A new and simple procedure for the determination of parathion in human whole blood and urine using direct immersion (DI) solid-phase microextraction (SPME) and gas chromatography/mass spectrometry (GC/MS) is presented. This technique was developed using only 100 ìL of sample, and ethion was used as internal standard (IS). A 65-ìm Carbowax/divinylbenzene (CW/DVB) SPME fibre was selected for sampling, and the main parameters affecting the SPME process such as extraction ...

  5. ZnO nanorod array solid phase micro-extraction fiber coating: fabrication and extraction capability

    International Nuclear Information System (INIS)

    Wang Dan; Zhang Zhuomin; Li Tiemei; Zhang Lan; Chen Guonan; Luo Lin

    2009-01-01

    In this paper, a ZnO nanorod array has been introduced as a coating to the headspace solid phase micro-extraction (HSSPME) field. The coating shows good extraction capability for volatile organic compounds (VOCs) by use of BTEX as a standard and can be considered suitable for sampling trace and small molecular VOC targets. In comparison with the randomly oriented ZnO nanorod HSSPME coating, ZnO nanorod array HSSPME fiber coating shows better extraction capability, which is attributed to the nanorod array structure of the coating. Also, this novel nanorod array coating shows good extraction selectivity to 1-propanethiol.

  6. Geometry of the vapor layer under a leidenfrost drop.

    Science.gov (United States)

    Burton, J C; Sharpe, A L; van der Veen, R C A; Franco, A; Nagel, S R

    2012-08-17

    In the Leidenfrost effect, liquid drops deposited on a hot surface levitate on a thin vapor cushion fed by evaporation of the liquid. This vapor layer forms a concave depression in the drop interface. Using laser-light interference coupled to high-speed imaging, we measured the radius, curvature, and height of the vapor pocket, as well as nonaxisymmetric fluctuations of the interface for water drops at different temperatures. The geometry of the vapor pocket depends primarily on the drop size and not on the substrate temperature.

  7. Oscillating and star-shaped drops levitated by an airflow.

    Science.gov (United States)

    Bouwhuis, Wilco; Winkels, Koen G; Peters, Ivo R; Brunet, Philippe; van der Meer, Devaraj; Snoeijer, Jacco H

    2013-08-01

    We investigate the spontaneous oscillations of drops levitated above an air cushion, eventually inducing a breaking of axisymmetry and the appearance of "star drops". This is strongly reminiscent of the Leidenfrost stars that are observed for drops floating above a hot substrate. The key advantage of this work is that we inject the airflow at a constant rate below the drop, thus eliminating thermal effects and allowing for a better control of the flow rate. We perform experiments with drops of different viscosities and observe stable states, oscillations, and chimney instabilities. We find that for a given drop size the instability appears above a critical flow rate, where the latter is largest for small drops. All these observations are reproduced by numerical simulations, where we treat the drop using potential flow and the gas as a viscous lubrication layer. Qualitatively, the onset of instability agrees with the experimental results, although the typical flow rates are too large by a factor 10. Our results demonstrate that thermal effects are not important for the formation of star drops and strongly suggest a purely hydrodynamic mechanism for the formation of Leidenfrost stars.

  8. Electromagnetic radiation due to nonlinear oscillations of a charged drop

    Science.gov (United States)

    Shiryaeva, S. O.; Grigor'ev, A. N.; Kolbneva, N. Yu.

    2016-03-01

    The nonlinear oscillations of a spherical charged drop are asymptotically analyzed under the conditions of a multimode initial deformation of its equilibrium shape. It is found that if the spectrum of initially excited modes contains two adjacent modes, the translation mode of oscillations is excited among others. In this case, the center of the drop's charge oscillates about the equilibrium position, generating a dipole electromagnetic radiation. It is shown that the intensity of this radiation is many orders of magnitude higher than the intensity of the drop's radiation, which arises in calculations of the first order of smallness and is related to the drop's charged surface oscillations.

  9. Improving BWR fuel critical power without increasing bundle pressure drop

    International Nuclear Information System (INIS)

    Matzner, B.; Shiraishi, L.M.; Danielson, D.W.; Congdon, S.P.

    2004-01-01

    It has been almost axiomatic that BWR fuel bundle critical power performance could not be improved without an accompanying increase in bundle pressure drop. It appeared that in order to increase the bundle dryout resistance it was necessary to perturb the bundle coolant flow paths in some fashion. This resulted in an unacceptable bundle pressure drop increase. However, by adding part length rods to decrease bundle pressure drop and by inserting an extra spacer with rearranged spacer pitch and flow trippers on the channel wall at the top of the bundle to increase critical power it was possible to achieve the goal of increased bundle critical power without pressure drop increase. (author)

  10. Multiresidue determination of pesticides from aquatic media using polyaniline nanowires network as highly efficient sorbent for microextraction in packed syringe.

    Science.gov (United States)

    Bagheri, Habib; Alipour, Noshin; Ayazi, Zahra

    2012-08-31

    A simple, rapid and sensitive method based on microextraction in packed syringe (MEPS), in combination with gas chromatography-mass spectrometry (GC-MS) was developed. Polyaniline (PANI) nanowires network was synthesized and used as sorbent of MEPS for the multiresidue determination of selected analytes from triazine, organochlrorine and organophosphorous pesticides in aqueous samples. The PANI nanowires network was prepared using soft template technique and its characterization was studied by scanning electron microscopy (SEM). The presence of micelles in this methodology showed to be an important parameter in shaping the growing polymer. Hexadecyltrimethylammonium bromide (HTAB) was used as structure directing agent in PANI preparation procedure and this was led to the formation of nanowires with diameters ranging from 35 nm to 45 nm. The synthesized PANI nanowires network showed higher extraction capability in comparison with the bulk PANI. Important parameters influencing the extraction and desorption processes including desorption solvent, elution volume, draw-eject cycles of sample, draw-eject mode, pH effect and amount of sorbent were optimized. Limits of detection were in the range of 0.07-0.3 ng mL(-1) using time scheduled selected ion monitoring (SIM) mode. The linearity of method was in the range from 0.5-200 ng mL(-1) to 0.2-1000 ng mL(-1). The method precision (RSD %) with three replicates were in the range of 5.3-18.4% at the concentration level of 5 ng mL(-1). The developed method was successfully applied to the Zayandeh-rood river water samples and the matrix factor obtained for the spiked real water samples were in the range of 0.79-0.94. Copyright © 2012 Elsevier B.V. All rights reserved.

  11. Ordered mesoporous carbon film as an effective solid-phase microextraction coating for determination of benzene series from aqueous media.

    Science.gov (United States)

    Jiang, Hui; Li, Jiansheng; Jiang, Mingyue; Lu, Rui; Shen, Jinyou; Sun, Xiuyun; Han, Weiqing; Wang, Lianjun

    2015-08-12

    The present work reports preparation of ordered mesoporous carbon (OMC) film supported on a graphite fiber as a new type of solid-phase microextraction (SPME) fiber for determination of benzene series from aqueous media. The strategy for the supported OMC film preparation was combined dip-coating technology with solvent evaporation-induced self-assembly (EISA) approach. A graphite fiber was immersed in an ethanol solution containing phenolic resin and Pluronic triblock copolymer. Upon solvent evaporation and subsequent pyrolysis under 700 °C, the phenolic resin and the surfactant self-assembled on the surface of the graphite fiber to form smooth OMC film. X-ray diffraction (XRD), transmission electron microscopy (TEM) and nitrogen isothermal adsorption results indicate that the resultant OMC film possesses well-ordered two dimensional hexagonal mesostructure with pore diameters of 4.5 nm and BET surfaces of 630 m(2)/g. Scanning electron microscopy (SEM) studies show the supported OMC film with thickness at 8.5 μm is continuous and defect-free. The SPME efficiency of the OMC fiber was evaluated by analysis of five benzene series (benzene, toluene, ethylbenzene, p-xylene and m-xylene) from water samples by gas chromatography-flame ionization detection (GC-FID). The analysis results indicate that the prepared OMC fiber has wide linear ranges (0.5-500 μg/L), low detection limits (0.01-0.05 μg/L) and good repeatabilities (4.0-5.8% for one fiber, 2.9-8.7% for fiber-to-fiber). Compared with commercial counterparts, the OMC fiber exhibits improved extraction efficiency for benzene series and PAHs. Copyright © 2015 Elsevier B.V. All rights reserved.

  12. Insights from the pollination drop proteome and the ovule transcriptome of Cephalotaxus at the time of pollination drop production.

    Science.gov (United States)

    Pirone-Davies, Cary; Prior, Natalie; von Aderkas, Patrick; Smith, Derek; Hardie, Darryl; Friedman, William E; Mathews, Sarah

    2016-05-01

    Many gymnosperms produce an ovular secretion, the pollination drop, during reproduction. The drops serve as a landing site for pollen, but also contain a suite of ions and organic compounds, including proteins, that suggests diverse roles for the drop during pollination. Proteins in the drops of species of Chamaecyparis, Juniperus, Taxus, Pseudotsuga, Ephedra and Welwitschia are thought to function in the conversion of sugars, defence against pathogens, and pollen growth and development. To better understand gymnosperm pollination biology, the pollination drop proteomes of pollination drops from two species of Cephalotaxus have been characterized and an ovular transcriptome for C. sinensis has been assembled. Mass spectrometry was used to identify proteins in the pollination drops of Cephalotaxus sinensis and C. koreana RNA-sequencing (RNA-Seq) was employed to assemble a transcriptome and identify transcripts present in the ovules of C. sinensis at the time of pollination drop production. About 30 proteins were detected in the pollination drops of both species. Many of these have been detected in the drops of other gymnosperms and probably function in defence, polysaccharide metabolism and pollen tube growth. Other proteins appear to be unique to Cephalotaxus, and their putative functions include starch and callose degradation, among others. Together, the proteins appear either to have been secreted into the drop or to occur there due to breakdown of ovular cells during drop production. Ovular transcripts represent a wide range of gene ontology categories, and some may be involved in drop formation, ovule development and pollen-ovule interactions. The proteome of Cephalotaxus pollination drops shares a number of components with those of other conifers and gnetophytes, including proteins for defence such as chitinases and for carbohydrate modification such as β-galactosidase. Proteins likely to be of intracellular origin, however, form a larger component of drops

  13. The Digital Drag and Drop Pillbox

    Science.gov (United States)

    Granger, Bradi B.; Locke, Susan C.; Bowers, Margaret; Sawyer, Tenita; Shang, Howard; Abernethy, Amy P.; Bloomfield, Richard A.; Gilliss, Catherine L.

    2017-01-01

    Objective: We present the design and feasibility testing for the “Digital Drag and Drop Pillbox” (D-3 Pillbox), a skill-based educational approach that engages patients and providers, measures performance, and generates reports of medication management skills. Methods: A single-cohort convenience sample of patients hospitalized with heart failure was taught pill management skills using a tablet-based D-3 Pillbox. Medication reconciliation was conducted, and aptitude, performance (% completed), accuracy (% correct), and feasibility were measured. Results: The mean age of the sample (n = 25) was 59 (36–89) years, 50% were women, 62% were black, 46% were uninsured, 46% had seventh-grade education or lower, and 31% scored very low for health literacy. However, most reported that the D-3 Pillbox was easy to read (78%), easy to repeat-demonstrate (78%), and comfortable to use (tablet weight) (75%). Accurate medication recognition was achieved by discharge in 98%, but only 25% reported having a “good understanding of my responsibilities.” Conclusions: The D-3 Pillbox is a feasible approach for teaching medication management skills and can be used across clinical settings to reinforce skills and medication list accuracy. PMID:28282304

  14. Career drop outs of young elite athletes

    Directory of Open Access Journals (Sweden)

    Petra Fišer

    2007-12-01

    Full Text Available The main problem of the study was to examine the characteristics of sports career drop outs of young elite sportswomen and their adaptation to the post-sport life. The sample included 20 ex-young elite sportswomen, who had brought their successful sport careers to an end before the age of 19. We used a modified interview about sports career termination (Cecić Erpič, 1998 for the investigation of the characteristics of their sports careers. To examine the caracteristics of sport careers we used frequency analysis and cluster analysis. The results showed that the participants mostly stated more than one reason for the termination of their career. The most common reasons for career termination were: lack of motivation, bad relations with trainers or co-competitors and dedication to school or education. After the end of a sports career most of the young sportswomen stayed actively in touch with sport, either as trainers, judges, or they remained engaged in sports for recreation.

  15. The viruses of wild pigeon droppings.

    Directory of Open Access Journals (Sweden)

    Tung Gia Phan

    Full Text Available Birds are frequent sources of emerging human infectious diseases. Viral particles were enriched from the feces of 51 wild urban pigeons (Columba livia from Hong Kong and Hungary, their nucleic acids randomly amplified and then sequenced. We identified sequences from known and novel species from the viral families Circoviridae, Parvoviridae, Picornaviridae, Reoviridae, Adenovirus, Astroviridae, and Caliciviridae (listed in decreasing number of reads, as well as plant and insect viruses likely originating from consumed food. The near full genome of a new species of a proposed parvovirus genus provisionally called Aviparvovirus contained an unusually long middle ORF showing weak similarity to an ORF of unknown function from a fowl adenovirus. Picornaviruses found in both Asia and Europe that are distantly related to the turkey megrivirus and contained a highly divergent 2A1 region were named mesiviruses. All eleven segments of a novel rotavirus subgroup related to a chicken rotavirus in group G were sequenced and phylogenetically analyzed. This study provides an initial assessment of the enteric virome in the droppings of pigeons, a feral urban species with frequent human contact.

  16. That's one small drop for Mankind...

    CERN Multimedia

    Anaïs Schaeffer

    2012-01-01

    In August, the members of an ISOLDE project called LOI88 successfully employed a new technique to study the interaction of metal ions in a liquid. It’s the first time that specific ions have been studied in a liquid medium - a technical achievement that opens promising doors for biochemistry.   In the heart of the LOI88 experiment: this is the point where the metal ions (from the left) enter the drop.  “More than half of the proteins in the human body contain metal ions such as magnesium, zinc and copper,” explains Monika Stachura, a biophysicist at the University of Copenhagen and the LOI88 project leader. “We know that these elements are crucial to a protein’s structure and function but their behaviour and interactions are not known in detail.” Detecting these ions directly in  a body-like environment is problematic as their closed atomic shells make them invisible to most spectroscopic techniques. However, using ...

  17. GENDER, DEBT, AND DROPPING OUT OF COLLEGE.

    Science.gov (United States)

    Dwyer, Rachel E; Hodson, Randy; McLoud, Laura

    2013-02-01

    For many young Americans, access to credit has become critical to completing a college education and embarking on a successful career path. Young people increasingly face the trade-off of taking on debt to complete college or foregoing college and taking their chances in the labor market without a college degree. These trade-offs are gendered by differences in college preparation and support and by the different labor market opportunities women and men face that affect the value of a college degree and future difficulties they may face in repaying college debt. We examine these new realities by studying gender differences in the role of debt in the pivotal event of graduating from college using the 1997 cohort of the national longitudinal Survey of youth. In this article, we find that women and men both experience slowing and even diminishing probabilities of graduating when carrying high levels of debt, but that men drop out at lower levels of debt than do women. We conclude by theorizing that high levels of debt are one of the mechanisms that sort women and men into different positions in the social stratification system.

  18. Dispersive solid-phase extraction followed by vortex-assisted dispersive liquid-liquid microextraction based on the solidification of a floating organic droplet for the determination of benzoylurea insecticides in soil and sewage sludge.

    Science.gov (United States)

    Peng, Guilong; He, Qiang; Mmereki, Daniel; Lu, Ying; Zhong, Zhihui; Liu, Hanyang; Pan, Weiliang; Zhou, Guangming; Chen, Junhua

    2016-04-01

    A novel dispersive solid-phase extraction combined with vortex-assisted dispersive liquid-liquid microextraction based on solidification of floating organic droplet was developed for the determination of eight benzoylurea insecticides in soil and sewage sludge samples before high-performance liquid chromatography with ultraviolet detection. The analytes were first extracted from the soil and sludge samples into acetone under optimized pretreatment conditions. Clean-up of the extract was conducted by dispersive solid-phase extraction using activated carbon as the sorbent. The vortex-assisted dispersive liquid-liquid microextraction based on solidification of floating organic droplet procedure was performed by using 1-undecanol with lower density than water as the extraction solvent, and the acetone contained in the solution also acted as dispersive solvent. Under the optimum conditions, the linearity of the method was in the range 2-500 ng/g with correlation coefficients (r) of 0.9993-0.9999. The limits of detection were in the range of 0.08-0.56 ng/g. The relative standard deviations varied from 2.16 to 6.26% (n = 5). The enrichment factors ranged from 104 to 118. The extraction recoveries ranged from 81.05 to 97.82% for all of the analytes. The good performance has demonstrated that the proposed methodology has a strong potential for application in the multiresidue analysis of complex matrices. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. Optimisation of ultrasound-assisted reverse micelles dispersive liquid-liquid micro-extraction by Box-Behnken design for determination of acetoin in butter followed by high performance liquid chromatography.

    Science.gov (United States)

    Roosta, Mostafa; Ghaedi, Mehrorang; Daneshfar, Ali

    2014-10-15

    A novel approach, ultrasound-assisted reverse micelles dispersive liquid-liquid microextraction (USA-RM-DLLME) followed by high performance liquid chromatography (HPLC) was developed for selective determination of acetoin in butter. The melted butter sample was diluted and homogenised by n-hexane and Triton X-100, respectively. Subsequently, 400μL of distilled water was added and the microextraction was accelerated by 4min sonication. After 8.5min of centrifugation, sedimented phase (surfactant-rich phase) was withdrawn by microsyringe and injected into the HPLC system for analysis. The influence of effective variables was optimised using Box-Behnken design (BBD) combined with desirability function (DF). Under optimised experimental conditions, the calibration graph was linear over the range of 0.6-200mgL(-1). The detection limit of method was 0.2mgL(-1) and coefficient of determination was 0.9992. The relative standard deviations (RSDs) were less than 5% (n=5) while the recoveries were in the range of 93.9-107.8%. Copyright © 2014. Published by Elsevier Ltd.

  20. Low pressure drop filtration of airborne molecular organic contaminants using open-channel networks

    Science.gov (United States)

    Dallas, Andrew J.; Joriman, Jon; Ding, Lefei; Weineck, Gerald; Seguin, Kevin

    2007-03-01

    Airborne molecular contamination (AMC) continues to play a very decisive role in the performance of many microelectronic devices and manufacturing processes. Besides airborne acids and bases, airborne organic contaminants such as 1-methyl-2-pyrrolidinone (NMP), hexamethyldisiloxane (HMDSO), trimethylsilanol (TMS), perfluoroalkylamines and condensables are of primary concern in these applications. Currently, the state of the filtration industry is such that optimum filter life and removal efficiency for organics is offered by granular carbon filter beds. However, the attributes that make packed beds of activated carbon extremely efficient also impart issues related to elevated filter weight and pressure drop. Most of the lower pressure drop AMC filters currently offered are quite expensive and are simply pleated combinations of various adsorptive and reactive media. On the other hand, low pressure drop filters, such as those designed as open-channel networks (OCN's), offer good filter life and removal efficiency with the additional benefits of significant reductions in overall filter weight and pressure drop. Equally important for many applications, the OCN filters can reconstruct the airflow so as to enhance the operation of a tool or process. For tool mount assemblies and fan filter units (FFUs) this can result in reduced fan and blower speeds, which subsequently can provide reduced vibration and energy costs. Additionally, these low pressure drop designs can provide a cost effective way of effectively removing AMC in full fab (or HVAC) filtration applications without significantly affecting air-handling requirements. Herein, we will present a new generation of low pressure drop OCN filters designed for the removal of airborne organics in a wide range of applications.

  1. Total sleep time severely drops during adolescence.

    Directory of Open Access Journals (Sweden)

    Damien Leger

    Full Text Available UNLABELLED: Restricted sleep duration among young adults and adolescents has been shown to increase the risk of morbidities such as obesity, diabetes or accidents. However there are few epidemiological studies on normal total sleep time (TST in representative groups of teen-agers which allow to get normative data. PURPOSE: To explore perceived total sleep time on schooldays (TSTS and non schooldays (TSTN and the prevalence of sleep initiating insomnia among a nationally representative sample of teenagers. METHODS: Data from 9,251 children aged 11 to 15 years-old, 50.7% of which were boys, as part of the cross-national study 2011 HBSC were analyzed. Self-completion questionnaires were administered in classrooms. An estimate of TSTS and TSTN (week-ends and vacations was calculated based on specifically designed sleep habits report. Sleep deprivation was estimated by a TSTN - TSTS difference >2 hours. Sleep initiating nsomnia was assessed according to International classification of sleep disorders (ICSD 2. Children who reported sleeping 7 hours or less per night were considered as short sleepers. RESULTS: A serious drop of TST was observed between 11 yo and 15 yo, both during the schooldays (9 hours 26 minutes vs. 7 h 55 min.; p<0.001 and at a lesser extent during week-ends (10 h 17 min. vs. 9 h 44 min.; p<0.001. Sleep deprivation concerned 16.0% of chidren aged of 11 yo vs. 40.5% of those of 15 yo (p<0.001. Too short sleep was reported by 2.6% of the 11 yo vs. 24.6% of the 15 yo (p<0.001. CONCLUSION: Despite the obvious need for sleep in adolescence, TST drastically decreases with age among children from 11 to 15 yo which creates significant sleep debt increasing with age.

  2. Application of dispersive liquid-liquid microextraction for the preconcentration of eight parabens in real samples and their determination by high-performance liquid chromatography.

    Science.gov (United States)

    Shen, Xiong; Liang, Jian; Zheng, Luxia; Lv, Qianzhou; Wang, Hong

    2017-11-01

    A simple and sensitive method for the simultaneous determination of eight parabens in human plasma and urine samples was developed. The samples were preconcentrated using dispersive liquid-liquid microextraction based on the solidification of floating organic drops and determined by high-performance liquid chromatography with ultraviolet detection. The influence of variables affecting the extraction efficiency was investigated and optimized using Placket-Burman design and Box-Behnken design. The optimized values were: 58 μL of 1-decanol (as extraction solvent), 0.65 mL methanol (as disperser solvent), 1.5% w/v NaCl in 5.0 mL of sample solution, pH 10.6, and 4.0 min centrifugation at 4000 rpm. The extract was injected into the high-performance liquid chromatography system for analysis. Under the optimum conditions, the linear ranges for eight parabens in plasma and urine were 1.0-1000 ng/mL, with correlation coefficients above 0.994. The limit of detection was 0.2-0.4 and 0.1-0.4 ng/mL for plasma and urine samples, respectively. Relative recoveries were between 80.3 and 110.7%, while relative standard deviations were less than 5.4%. Finally, the method was applied to analyze the parabens in 98 patients of primary breast cancer. Results showed that parabens existed widely, at least one paraben detected in 96.9% (95/98) of plasma samples and 98.0% (96/98) of urine samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Automation of static and dynamic non-dispersive liquid phase microextraction. Part 2: Approaches based on impregnated membranes and porous supports.

    Science.gov (United States)

    Alexovič, Michal; Horstkotte, Burkhard; Solich, Petr; Sabo, Ján

    2016-02-11

    A critical overview on automation of modern liquid phase microextraction (LPME) approaches based on the liquid impregnation of porous sorbents and membranes is presented. It is the continuation of part 1, in which non-dispersive LPME techniques based on the use of the extraction phase (EP) in the form of drop, plug, film, or microflow have been surveyed. Compared to the approaches described in part 1, porous materials provide an improved support for the EP. Simultaneously they allow to enlarge its contact surface and to reduce the risk of loss by incident flow or by components of surrounding matrix. Solvent-impregnated membranes or hollow fibres are further ideally suited for analyte extraction with simultaneous or subsequent back-extraction. Their use can therefore improve the procedure robustness and reproducibility as well as it "opens the door" to the new operation modes and fields of application. However, additional work and time are required for membrane replacement and renewed impregnation. Automation of porous support-based and membrane-based approaches plays an important role in the achievement of better reliability, rapidness, and reproducibility compared to manual assays. Automated renewal of the extraction solvent and coupling of sample pretreatment with the detection instrumentation can be named as examples. The different LPME methodologies using impregnated membranes and porous supports for the extraction phase and the different strategies of their automation, and their analytical applications are comprehensively described and discussed in this part. Finally, an outlook on future demands and perspectives of LPME techniques from both parts as a promising area in the field of sample pretreatment is given. Copyright © 2015 Elsevier B.V. All rights reserved.

  4. Microextraction Techniques Used in the Procedures for Determining Organomercury and Organotin Compounds in Environmental Samples

    Directory of Open Access Journals (Sweden)

    Małgorzata Rutkowska

    2014-06-01

    Full Text Available Due to human activities, the concentrations of organometallic compounds in all parts of the environment have increased in recent decades. The toxicity and some biochemical properties of mercury and tin present in the environment depend on the concentration and chemical form of these two elements. The ever-increasing demand for determining compounds at very low concentration levels in samples with complex matrices requires the elimination of interfering substances, the reduction of the final extract volume, and analyte enrichment in order to employ a detection technique, which is characterised by high sensitivity at low limits of quantification. On the other hand, in accordance with current trends, the analytical procedures should aim at the miniaturisation and simplification of the sample preparation step. In the near future, more importance will be given to the fulfilment of the requirements of Green Chemistry and Green Analytical Chemistry in order to reduce the intensity of anthropogenic activities related to analytical laboratories. In this case, one can consider the use of solvent-free/solvent-less techniques for sample preparation and microextraction techniques, because the use of the latter leads to lowering the quantity of reagents used (including solvents due to the reduction of the scale of analysis. This paper presents an overview of microextraction techniques (SPME and LPME used in the procedures for determining different chemical forms of mercury and tin.

  5. A star-shaped polythiophene dendrimer coating for solid-phase microextraction of triazole agrochemicals.

    Science.gov (United States)

    Abolghasemi, Mir Mahdi; Habibiyan, Rahim; Jaymand, Mehdi; Piryaei, Marzieh

    2018-02-14

    A nanostructured star-shaped polythiophene dendrimer was prepared and used as a fiber coating for headspace solid phase microextraction of selected triazolic pesticides (tebuconazole, hexaconazole, penconazole, diniconazole, difenoconazole, triticonazole) from water samples. The dendrimer with its large surface area was characterized by thermogravimetric analysis, UV-Vis spectroscopy and field emission scanning electron microscopy. It was placed on a stainless steel wire for use in SPME. The experimental conditions for fiber coating, extraction, stirring rate, ionic strength, pH value, desorption temperature and time were optimized. Following thermal desorption, the pesticides were quantified by GC-MS. Under optimum conditions, the repeatability (RSD) for one fiber (for n = 3) ranges from 4.3 to 5.6%. The detection limits are between 8 and 12 pg mL -1 . The method is fast, inexpensive (in terms of equipment), and the fiber has high thermal stability. Graphical abstract Schematic presentation of a nanostructured star-shaped polythiophene dendrimer for use in headspace solid phase microextraction of the triazolic pesticides (tebuconazole, hexaconazole, penconazole, diniconazole, difenoconazole, triticonazole). They were then quantified by gas chromatography-mass spectrometry.

  6. Silicon carbide nanomaterial as a coating for solid-phase microextraction.

    Science.gov (United States)

    Tian, Yu; Feng, Juanjuan; Wang, Xiuqin; Sun, Min; Luo, Chuannan

    2018-01-26

    Silicon carbide has excellent properties, such as corrosion resistance, high strength, oxidation resistance, high temperature, and so on. Based on these properties, silicon carbide was coated on stainless-steel wire and used as a solid-phase microextraction coating, and polycyclic aromatic hydrocarbons were employed as model analytes. Using gas chromatography, some important factors that affect the extraction efficiency were optimized one by one, and an analytical method was established. The analytical method showed wide linear ranges (0.1-30, 0.03-30, and 0.01-30 μg/L) with satisfactory correlation coefficients (0.9922-0.9966) and low detection limits (0.003-0.03 μg/L). To investigate the practical application of the method, rainwater and cigarette ash aqueous solution were collected as real samples for extraction and detection. The results indicate that silicon carbide has excellent application in the field of solid-phase microextraction. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Graphene-functionalized melamine sponges for microextraction of sulfonamides from food and environmental samples.

    Science.gov (United States)

    Chatzimitakos, Theodoros; Samanidou, Victoria; Stalikas, Constantine D

    2017-11-03

    The study describes the functionalization of melamine sponges with graphene and its use as an adsorbent for the microextraction of sulfonamides from food and environmental samples. The graphene-functionalized melamine sponge (GMeS) was prepared by an easy, one-step procedure, which complies with the principles of green chemistry and is proved advantageous over previously described methods. The applicability of the GMeS in extraction procedures was studied and an analytical method for the determination of sulfonamides in milk, eggs and lake water was developed and validated according to SANCO/12571/2013 guideline. The developed method was highly accurate and reproducible, while the limits of quantification were found to be relatively low (0.31-0.91μgkg -1 , 0.96-1.32μgkg -1 and 0.10-0.29μgL -1 in the case of milk, eggs and lake water respectively). Furthermore, matrix effects were absent in all cases, since the microextraction procedure serves also as a clean-up step. The low cost of synthesis, the environmentally friendly conditions, the efficiency and high extraction recoveries are some additional advantages of the proposed procedure. To the best of our knowledge, this is the first time that a GMeS is prepared in a straightforward way and used for analytical purposes. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. Recent developments and future trends in solid phase microextraction techniques towards green analytical chemistry.

    Science.gov (United States)

    Spietelun, Agata; Marcinkowski, Łukasz; de la Guardia, Miguel; Namieśnik, Jacek

    2013-12-20

    Solid phase microextraction find increasing applications in the sample preparation step before chromatographic determination of analytes in samples with a complex composition. These techniques allow for integrating several operations, such as sample collection, extraction, analyte enrichment above the detection limit of a given measuring instrument and the isolation of analytes from sample matrix. In this work the information about novel methodological and instrumental solutions in relation to different variants of solid phase extraction techniques, solid-phase microextraction (SPME), stir bar sorptive extraction (SBSE) and magnetic solid phase extraction (MSPE) is presented, including practical applications of these techniques and a critical discussion about their advantages and disadvantages. The proposed solutions fulfill the requirements resulting from the concept of sustainable development, and specifically from the implementation of green chemistry principles in analytical laboratories. Therefore, particular attention was paid to the description of possible uses of novel, selective stationary phases in extraction techniques, inter alia, polymeric ionic liquids, carbon nanotubes, and silica- and carbon-based sorbents. The methodological solutions, together with properly matched sampling devices for collecting analytes from samples with varying matrix composition, enable us to reduce the number of errors during the sample preparation prior to chromatographic analysis as well as to limit the negative impact of this analytical step on the natural environment and the health of laboratory employees. Copyright © 2013 Elsevier B.V. All rights reserved.

  9. Detection of bubble nucleation event in superheated drop detector ...

    Indian Academy of Sciences (India)

    2016-12-08

    Dec 8, 2016 ... Superheated drop detector consisting of drops of superheated liquid suspended in polymer or gel matrix is of great demand, mainly ... ing to which as the radiation deposits energy along its path inside the superheated liquid, ... resistance with change in pressure in a system. The frequency response of the ...

  10. Why Did They Not Drop Out? Narratives from Resilient Students

    Science.gov (United States)

    Lessard, Anne; Fortin, Laurier; Marcotte, Diane; Potvin, Pierre; Royer, Egide

    2009-01-01

    There is much to be learned from students who were at-risk for dropping out of school but persevered and graduated. The purpose of the study on which this article is based, was to describe how students who were at-risk for dropping out of school persevered and graduated. The voices of two students are introduced, highlighting the challenges they…

  11. SAW-controlled drop size for flow focusing.

    Science.gov (United States)

    Schmid, Lothar; Franke, Thomas

    2013-05-07

    We demonstrate the regularization of droplet formation by applying a surface acoustic wave (SAW) localized at the flow-focus junction of a drop maker. This allows electronic control of drop size in real time, without changing the flow rates or microchannel dimensions.

  12. Vortex Shedding and Depinning of Wind-Forced Liquid Drops

    Science.gov (United States)

    Simon, Roger; White, Edward

    2017-11-01

    Water drops adhere to solid substrates but can depin when wind forcing exceeds the adhesion force provided by surface tension. Schmucker and White (2012.DFD.M4.6) measured critical wind forcing limits for high-Reynolds-number airflow forcing and found a critical constant Weber number, Wecrit = 8.0 , for a range of drop Bond numbers. This work seeks to identify what behavior is associated with Wecrit = 8.0 and why wind-forced drops depin when they do. One hypothesis suggests that, at high Reynolds numbers, drops depin when their interface natural frequency matches the frequency of air vortex shedding in the separated drop wake. We investigate whether a resonance between vortex shedding and drop interface oscillations is involved with depinning. We measure the shedding frequencies behind solid protuberances of the same size as typical drops and, separately, water-drop interface frequencies. We compare our measured values under different flow conditions to establish whether shedding and interface resonance are related to depinning. 1Supported by the National Science Foundation through Grant CBET-1605947.

  13. 14 CFR 23.725 - Limit drop tests.

    Science.gov (United States)

    2010-01-01

    ... used in the drop test (lbs.); h=specified free drop height (inches); d=deflection under impact of the tire (at the approved inflation pressure) plus the vertical component of the axle travel relative to... must be made on the complete airplane, or on units consisting of wheel, tire, and shock absorber, in...

  14. Evaluation of Sodium Sulphacetamide drops in the Treatment of ...

    African Journals Online (AJOL)

    Sodium sulphacetamide eye drops had been used successfully in the past in the treatment of ophthalmia neonatorium (ON) but its use has decreased remarkably in recent time. The efficacy of 10 percent sodium sulphacetamide eye drops in the treatment of ON was prospectively evaluated in 68 neonates seen in our ...

  15. Student Drop-Out from German Higher Education Institutions

    Science.gov (United States)

    Heublein, Ulrich

    2014-01-01

    28% of students of any one year currently give up their studies in bachelor degree programmes at German higher education institutions. Drop-out is to be understood as the definite termination in the higher education system without obtaining an academic degree. The drop-out rate is thereby calculated with the help of statistical estimation…

  16. Complex cooling water systems optimization with pressure drop consideration

    CSIR Research Space (South Africa)

    Gololo, KV

    2012-12-01

    Full Text Available Pressure drop consideration has shown to be an essential requirement for the synthesis of a cooling water network where reuse/recycle philosophy is employed. This is due to an increased network pressure drop associated with additional reuse...

  17. Reconfigurable Optical Add-Drop Multiplexer Using Microring Resonators

    NARCIS (Netherlands)

    Klein, E.J.; Geuzebroek, D.H.; Kelderman, H.; Sengo, G.; Sengo, G.; Baker, Nigel; Driessen, A.

    2005-01-01

    We report a reconfigurable four-channel optical add–drop multiplexer for use in access networks. The optical add–drop multiplexer (OADM) is based on vertically coupled thermally tunable $Si_3N_4$ – $SiO_2$ microring resonators (MRs) and has been realized on a footprint of 0.25 mm2. Individual MRs in

  18. Drop shape visualization and contact angle measurement on curved surfaces.

    Science.gov (United States)

    Guilizzoni, Manfredo

    2011-12-01

    The shape and contact angles of drops on curved surfaces is experimentally investigated. Image processing, spline fitting and numerical integration are used to extract the drop contour in a number of cross-sections. The three-dimensional surfaces which describe the surface-air and drop-air interfaces can be visualized and a simple procedure to determine the equilibrium contact angle starting from measurements on curved surfaces is proposed. Contact angles on flat surfaces serve as a reference term and a procedure to measure them is proposed. Such procedure is not as accurate as the axisymmetric drop shape analysis algorithms, but it has the advantage of requiring only a side view of the drop-surface couple and no further information. It can therefore be used also for fluids with unknown surface tension and there is no need to measure the drop volume. Examples of application of the proposed techniques for distilled water drops on gemstones confirm that they can be useful for drop shape analysis and contact angle measurement on three-dimensional sculptured surfaces. Copyright © 2011 Elsevier Inc. All rights reserved.

  19. The origin of star-shaped oscillations of Leidenfrost drops

    Science.gov (United States)

    Ma, Xiaolei; Burton, Justin C.

    We experimentally investigate the oscillations of Leidenfrost drops of water, liquid nitrogen, ethanol, methanol, acetone and isopropyl alcohol. The drops levitate on a cushion of evaporated vapor over a hot, curved surface which keeps the drops stationary. We observe star-shaped modes along the periphery of the drop, with mode numbers n = 2 to 13. The number of observed modes is sensitive to the properties of the liquid. The pressure oscillation frequency in the vapor layer under the drop is approximately twice that of the drop frequency, which is consistent with a parametric forcing mechanism. However, the Rayleigh and thermal Marangoni numbers are of order 10,000, indicating that convection should play a dominating role as well. Surprisingly, we find that the wavelength and frequency of the oscillations only depend on the thickness of the liquid, which is twice the capillary length, and do not depend on the mode number, substrate temperature, or the substrate curvature. This robust behavior suggests that the wavelength for the oscillations is set by thermal convection inside the drop, and is less dependent on the flow in the vapor layer under the drop

  20. Simulation of the drop impact test for moulded thermoplastic containers

    NARCIS (Netherlands)

    Reed, P.E.; Breedveld, G.; Lim, B.C.

    2000-01-01

    An analysis is made of the drop impact test for moulded plastics containers, as a first step towards the simulation of the impact event for design and development purposes. Experimental data are analysed from instrumented base drop impact testing of water-filled blow-moulded bottles, 20 and 210 l

  1. Capillary-inertial colloidal catapults upon drop coalescence

    Science.gov (United States)

    Chen, Chuan-Hua

    2016-01-01

    Surface energy released upon drop coalescence is known to power the self-propelled jumping of liquid droplets on superhydrophobic solid surfaces, and the jumping droplets can additionally carry colloidal payloads toward self-cleaning. Here, we show that drop coalescence on a spherical particle leads to self-propelled launching of the particle from virtually any solid surface. The main prerequisite is an intermediate wettability of the particle, such that the momentum from the capillary-inertial drop coalescence process can be transferred to the particle. By momentum conservation, the launching velocity of the particle-drop complex is proportional to the capillary-inertial velocity based on the drop radius and to the fraction of the liquid mass in the total mass. The capillary-inertial catapult is not only an alternative mechanism for removing colloidal contaminants, but also a useful model system for studying ballistospore launching. PMID:27478201

  2. Silicon wavelength-selective partial-drop broadcast filter bank.

    Science.gov (United States)

    Su, Zhan; Cherchi, Matteo; Timurdogan, Erman; Sun, Jie; Moresco, Michele; Leake, Gerald; Coolbaugh, Douglas; Watts, Michael R

    2014-09-15

    We propose an approach to a wavelength-selective 1×N port optical broadcast network demonstrating the approach in a 1×8 port parallel optical drop filter bank utilizing adiabatic micro-ring tunable filters. The micro-ring filters exhibit first-order 92.7±3.7 GHz full width at half-maximum bandwidths with a 36.2 nm free spectral range, low-drop power variation (0.11 dB), and aggregate excess loss of only 1.1 dB in all drop ports. Error-free operation at a 10 Gbit/s data rate is achieved for all eight drop ports with less than a 0.5 dB power penalty among the ports. This wavelength-selective parallel-drop approach serves as a building block for on-chip all-to-all communication networks.

  3. Drop tests of the Three Mile Island knockout canister

    International Nuclear Information System (INIS)

    Box, W.D.; Aaron, W.S.; Shappert, L.B.; Childress, P.C.; Quinn, G.J.; Smith, J.V.

    1987-01-01

    A type of Three Mile Island Unit 2 (TMI-2) defueling canister, called a ''knockout'' canister, was subjected to a series of drop tests at the Oak Ridge National Laboratory's Drop Test Facility. These tests confirmed the structural integrity of internal fixed neutron poisons in support of a request for NRC licensing of this type of canister for the shipment of TMI-2 reactor fuel debris to the Idaho National Engineering Laboratory (INEL) for the Core Examination R and D Program. This report presents the data generated and the results obtained from a series of four drop tests that included two drops with the test assembly in the vertical position and two drops with the assembly in the horizontal position

  4. About applicability of thermodynamic parameters to small drops and clusters

    Science.gov (United States)

    Kharlamov, G. V.; Onischuk, A. A.; Vosel, S. V.; Purtov, P. A.

    2012-11-01

    In our paper the results of molecular dynamics calculations of nanodrops are presented. The density profiles, the Irving-Kirkwood pressure tensors, the chemical potentials of the systems, the equimolar radii of the drops and the radii of tension, the mechanical and thermodynamic surface tensions have been calculated. It is shown that both the mechanical and thermodynamic surface tensions decrease with the decrease of the equimolar radius of the drop and reach zero at the same R0 depending on temperature. With the further equimolar radius decrease the surface tension becomes negative. It means that such droplet is metastable and that the notion of the macroscopic surface tension cannot be applied to such small drops. The dependence of the ratio of the drop surface tension to the surface tension of the flat liquid-vapor interface on the ratio of the drop equimolar radius to R0 is a universal function.

  5. About applicability of thermodynamic parameters to small drops and clusters

    International Nuclear Information System (INIS)

    Kharlamov, G V; Onischuk, A A; Vosel, S V; Purtov, P A

    2012-01-01

    In our paper the results of molecular dynamics calculations of nanodrops are presented. The density profiles, the Irving-Kirkwood pressure tensors, the chemical potentials of the systems, the equimolar radii of the drops and the radii of tension, the mechanical and thermodynamic surface tensions have been calculated. It is shown that both the mechanical and thermodynamic surface tensions decrease with the decrease of the equimolar radius of the drop and reach zero at the same R 0 depending on temperature. With the further equimolar radius decrease the surface tension becomes negative. It means that such droplet is metastable and that the notion of the macroscopic surface tension cannot be applied to such small drops. The dependence of the ratio of the drop surface tension to the surface tension of the flat liquid-vapor interface on the ratio of the drop equimolar radius to R 0 is a universal function.

  6. Building micro-soccer-balls with evaporating colloidal fakir drops

    Science.gov (United States)

    Gelderblom, Hanneke; Marín, Álvaro G.; Susarrey-Arce, Arturo; van Housselt, Arie; Lefferts, Leon; Gardeniers, Han; Lohse, Detlef; Snoeijer, Jacco H.

    2013-11-01

    Drop evaporation can be used to self-assemble particles into three-dimensional microstructures on a scale where direct manipulation is impossible. We present a unique method to create highly-ordered colloidal microstructures in which we can control the amount of particles and their packing fraction. To this end, we evaporate colloidal dispersion drops from a special type of superhydrophobic microstructured surface, on which the drop remains in Cassie-Baxter state during the entire evaporative process. The remainders of the drop consist of a massive spherical cluster of the microspheres, with diameters ranging from a few tens up to several hundreds of microns. We present scaling arguments to show how the final particle packing fraction of these balls depends on the drop evaporation dynamics, particle size, and number of particles in the system.

  7. Microextraction Techniques Coupled to Liquid Chromatography with Mass Spectrometry for the Determination of Organic Micropollutants in Environmental Water Samples

    Directory of Open Access Journals (Sweden)

    Mª Esther Torres Padrón

    2014-07-01

    Full Text Available Until recently, sample preparation was carried out using traditional techniques, such as liquid–liquid extraction (LLE, that use large volumes of organic solvents. Solid-phase extraction (SPE uses much less solvent than LLE, although the volume can still be significant. These preparation methods are expensive, time-consuming and environmentally unfriendly. Recently, a great effort has been made to develop new analytical methodologies able to perform direct analyses using miniaturised equipment, thereby achieving high enrichment factors, minimising solvent consumption and reducing waste. These microextraction techniques improve the performance during sample preparation, particularly in complex water environmental samples, such as wastewaters, surface and ground waters, tap waters, sea and river waters. Liquid chromatography coupled to tandem mass spectrometry (LC/MS/MS and time-of-flight mass spectrometric (TOF/MS techniques can be used when analysing a broad range of organic micropollutants. Before separating and detecting these compounds in environmental samples, the target analytes must be extracted and pre-concentrated to make them detectable. In this work, we review the most recent applications of microextraction preparation techniques in different water environmental matrices to determine organic micropollutants: solid-phase microextraction SPME, in-tube solid-phase microextraction (IT-SPME, stir bar sorptive extraction (SBSE and liquid-phase microextraction (LPME. Several groups of compounds are considered organic micropollutants because these are being released continuously into the environment. Many of these compounds are considered emerging contaminants. These analytes are generally compounds that are not covered by the existing regulations and are now detected more frequently in different environmental compartments. Pharmaceuticals, surfactants, personal care products and other chemicals are considered micropollutants. These

  8. Effect of formulation factors on in vitro transcorneal permeation of voriconazole from aqueous drops

    Directory of Open Access Journals (Sweden)

    Biswaranjan Mohanty

    2013-01-01

    Full Text Available The purpose of this research was to evaluate the effect the formulation factors on in vitro permeation of voriconazole through freshly isolated goat and sheep corneas. An increase in the pH of the drops from 4.0 to 8.0 resulted in significant (P < 0.05 increase drug permeation. Raising concentration of the drops from 0.05% to 0.2% (w/v significantly, (P < 0.05 increased drug permeation, but decreased the percent permeation. Corneal transport of voriconazole is both pH and concentration dependent. Eye drops containing disodium edetate (ethylenediaminetetraacetic acid alone or combination with benzalkonium chloride showed significantly (P < 0.05 higher permeation as compared with control formulation. Addition of beta-cyclodextrin to the formulation enhanced corneal permeation of voriconazole. Compared with control formulation, voriconazole 0.2% (w/v drop containing viscosity modifier produced significant (P < 0.05 decrease in permeation. Most of the formulations showed higher zone of inhibition against Candida albicans.

  9. In Vitro Evaluation of the Ophthalmic Toxicity Profile of Chlorhexidine and Propamidine Isethionate Eye Drops.

    Science.gov (United States)

    Fernández-Ferreiro, Anxo; Santiago-Varela, María; Gil-Martínez, María; González-Barcia, Miguel; Luaces-Rodríguez, Andrea; Díaz-Tome, Victoria; Pardo, María; Méndez, José Blanco; Piñeiro-Ces, Antonio; Rodríguez-Ares, María Teresa; Lamas, Maria Jesus; Otero-Espinar, Francisco J

    2017-04-01

    Acanthamoeba keratitis causes frequent epithelial lesions that fully expose the corneal stroma. The aim of this study was to determine the toxic profile of chlorhexidine and propamidine eye drops. We used primary human keratocytes in cell culture in combination with a novel technology that evaluates dynamic real-time cytotoxicity through impedance analysis. Additional studies such as a classic cell viability test (WST-1 ® ), a bovine corneal opacity and permeability assay, and an irritation eye study (Hen's Egg Test [HET]) have been made. Both eye drop formulations showed a time- and concentration-dependent toxicity profile, in which long periods and high concentrations were more detrimental to cells. In prolonged times of exposure, propamidine is more harmful to cells than chlorhexidine. On the contrary, no irritation has been detected in using the HET-chorioallantoic membrane test and no alterations in the corneal transparency nor permeability was produced by the treatment with both eye drops. In culture assay, chlorhexidine eye drops have proven to be less cytotoxic than Brolene ® for a long contact period of time, but no signs of irritation or alterations in transparency or permeability have been observed in the cornea after both treatments.

  10. Formulation of indomethacin eye drops via complexation with cyclodextrins.

    Science.gov (United States)

    Halim Mohamed, Maaly A; Mahmoud, Azza A

    2011-03-01

    Topically administered indomethacin is used in the management and prevention of ocular inflammation and cystoid macular edema related to cataract surgery and in the maintenance of mydriasis during cataract surgery. Pharmaceutically, the main obstacle in formulating indomethacin as eye drops is its low solubility and aqueous instability. Inclusion complexation of indomethacin with cyclodextrins (CDs) was our interest in this research to obtain stable and effective aqueous indomethacin eye drops. The influence of β-CD, hydroxypropyl-β-CD (HP-β-CD), and sulfobutyl ether-β-CD (SBE-β-CD) on indomethacin solubility was investigated. Indomethacin-HP-β-CD complex was prepared and characterized by infrared spectroscopy, differential scanning calorimetry, and X-ray diffractometry and was subjected to in vitro release and stability studies. The anti-inflammatory effect of formulated indomethacin-HP-β-CD eye drops on chemically burned albino rabbit eyes was compared to those of Indocollyre(®) and Voltaren(®) eye drops. HP-β-CD was found to have a high solubilizing effect towards indomethacin and was thus selected for its formulation. Formulated indomethacin-HP-β-CD eye drops exhibited delayed release and high drug stability compared to the drug solution. Draize rabbit eye irritation test and histological examination on albino rabbit eyes treated with indomethacin-HP-β-CD eye drops revealed that these eye drops were non-irritant. The anti-inflammatory studies indicated that formulating indomethacin eye drops via complexation with HP-β-CD significantly improves the therapeutic efficacy of the indomethacin compared to the investigated eye drops. An aqueous ocular delivery system for the poor water soluble anti-inflammatory indomethacin was prepared using HP-β-CD as a complexing agent. Besides a sufficient solubility for the drug, many factors were studied in the development of this system, such as stability and safety. In addition, indomethacin-HP-β-CD eye drops

  11. Proton radioactivity within a generalized liquid drop model

    Science.gov (United States)

    Dong, J. M.; Zhang, H. F.; Royer, G.

    2009-05-01

    The proton radioactivity half-lives of spherical proton emitters are investigated theoretically. The potential barriers preventing the emission of protons are determined in the quasimolecular shape path within a generalized liquid drop model (GLDM) including the proximity effects between nuclei in a neck and the mass and charge asymmetry. The penetrability is calculated with the WKB approximation. The spectroscopic factor has been taken into account in half-life calculation, which is obtained by employing the relativistic mean field (RMF) theory combined with the BCS method with the force NL3. The half-lives within the GLDM are compared with the experimental data and other theoretical values. The GLDM works quite well for spherical proton emitters when the spectroscopic factors are considered, indicating the necessity of introducing the spectroscopic factor and the success of the GLDM for proton emission. Finally, we present two formulas for proton emission half-life calculation similar to the Viola-Seaborg formulas and Royer's formulas of α decay.

  12. SIMPLE METHOD FOR ESTIMATING POLYCHLORINATED BIPHENYL CONCENTRATIONS ON SOILS AND SEDIMENTS USING SUBCRITICAL WATER EXTRACTION COUPLED WITH SOLID-PHASE MICROEXTRACTION. (R825368)

    Science.gov (United States)

    A rapid method for estimating polychlorinated biphenyl (PCB) concentrations in contaminated soils and sediments has been developed by coupling static subcritical water extraction with solid-phase microextraction (SPME). Soil, water, and internal standards are placed in a seale...

  13. Separation and preconcentration system based on microextraction with ionic liquid for determination of copper in water and food samples by stopped-flow injection spectrofluorimetry.

    Science.gov (United States)

    Zeeb, Mohsen; Ganjali, Mohammad Reza; Norouzi, Parviz; Kalaee, Mohamad Reza

    2011-05-01

    In this work, an efficient in situ solvent formation microextraction (ISFME) was combined with stopped-flow injection spectrofluorimetry (SFIS) for the determination of copper. In the proposed approach, thiamine was oxidized with copper(II) to form hydrophobic and highly fluorescent thiochrome (TC), which was subsequently extracted into ionic liquid as an extractant phase. A small amount of an ion-pairing agent (NaPF(6)) was added to the sample solution containing a water-miscible ionic liquid ([Hmim][BF(4)]) to obtain a hydrophobic ionic liquid ([Hmim][PF(6)]), which acted as the extraction phase. After centrifuging, phase separation was performed and the enriched analyte was determined by SFIS. ISFME is an efficient method for separation and preconcentration of metal ions from aqueous solutions with a high ionic strength. Variables affecting the analytical performance were studied and optimized. Under optimum experimental conditions, the proposed method provided a limit of detection (LOD) of 0.024μgL(-1) and a relative standard deviation (RSD) of 2.1%. The accuracy of the combined methodology was evaluated by recovery experiments and by analyzing certified reference material (GBW 07605 Tea). Finally, the proposed method was successfully applied to copper determination in water and food samples. Copyright © 2011 Elsevier Ltd. All rights reserved.

  14. Calculation of water drop trajectories to and about arbitrary three-dimensional lifting and nonlifting bodies in potential airflow

    Science.gov (United States)

    Norment, H. G.

    1985-01-01

    Subsonic, external flow about nonlifting bodies, lifting bodies or combinations of lifting and nonlifting bodies is calculated by a modified version of the Hess lifting code. Trajectory calculations can be performed for any atmospheric conditions and for all water drop sizes, from the smallest cloud droplet to large raindrops. Experimental water drop drag relations are used in the water drop equations of motion and effects of gravity settling are included. Inlet flow can be accommodated, and high Mach number compressibility effects are corrected for approximately. Seven codes are described: (1) a code used to debug and plot body surface description data; (2) a code that processes the body surface data to yield the potential flow field; (3) a code that computes flow velocities at arrays of points in space; (4) a code that computes water drop trajectories from an array of points in space; (5) a code that computes water drop trajectories and fluxes to arbitrary target points; (6) a code that computes water drop trajectories tangent to the body; and (7) a code that produces stereo pair plots which include both the body and trajectories. Accuracy of the calculations is discussed, and trajectory calculation results are compared with prior calculations and with experimental data.

  15. Transient dynamics of confined liquid drops in a uniform electric field

    Science.gov (United States)

    Mandal, Shubhadeep; Chaudhury, Kaustav; Chakraborty, Suman

    2014-05-01

    We analyze the effect of confinement on the transient dynamics of liquid drops, suspended in another immiscible liquid medium, under the influence of an externally applied uniform dc electric field. For our analysis, we adhere to an analytical framework conforming to a Newtonian-leaky-dielectric liquid model in the Stokes flow regime, under the small deformation approximation. We characterize the transient relaxation of the drop shape towards its asymptotic configuration, attributed by the combined confluence of the charge-relaxation time scale and the intrinsic shape-relaxation time scale. While the former appears due to the charge accumulation process on the drop surface over a finite interval of time, the genesis of the latter is found to be intrinsic to the hydrodynamic situation under consideration. In an unbounded condition, the intrinsic shape-relaxation time scale is strongly governed by the viscosity ratio, defined as the ratio of dynamic viscosities of the droplet and the background liquid. However, when the wall effects are brought into consideration, the combined influence of the relative extent of the confinement and the intrinsic viscosity effects, acting in tandem, alter this time scale in a rather complicated and nontrivial manner. We reveal that the presence of confinement may dramatically increase the effective viscosity ratio that could have otherwise been required in an unconfined domain to realize identical time-relaxation characteristics. We also bring out the alterations in the streamline patterns because of the combinations of transient and confinement effects. Thus, our results reveal that the extent of fluidic confinement may provide an elegant alternative towards manipulating the transient dynamics of liquid drops in the presence of an externally applied electric field, bearing far-ranging consequences towards the design and functionalities of several modern-day microfluidic applications.

  16. Effect of humidity on the filter pressure drop

    International Nuclear Information System (INIS)

    Vendel, J.; Letourneau, P.

    1995-01-01

    The effects of humidity on the filter pressure drop have been reported in some previous studies in which it is difficult to draw definite conclusions. These studies show contradictory effects of humidity on the pressure drop probably due to differences in the hygroscopicity of the test aerosols. The objective of this paper is to present experimental results on the evolution of the filter pressure drop versus mass loading, for different test aerosols and relative humidities. Present results are compared to those found in various publication. An experimental device has been designed to measure filter pressure drop as the function of the areal density for relative humidity varying in the range of 9 % to 85 %. Experiments have been conducted with hygroscopic: (CsOH) and nonhygroscopic aerosols (TiO 2 ). Cesium hydroxyde (CsOH) of size of 2 μ M AMMD has been generated by an ultrasonic generator and the 0.7 μm AMMD titanium oxyde has been dispersed by a open-quotes turn-tableclose quotes generator. As it is noted in the BISWAS'publication [3], present results show, in the case of nonhygroscopic aerosols, a linear relationship of pressure drop to mass loading. For hygroscopic aerosols two cases must be considered: for relative humidity below the deliquescent point of the aerosol, the relationship of pressure drop to mass loading remains linear; above the deliquescent point, the results show a sudden increase in the pressure drop and the mass capacity of the filter is drastically reduced

  17. Effect of humidity on the filter pressure drop

    Energy Technology Data Exchange (ETDEWEB)

    Vendel, J.; Letourneau, P. [Institut de Protection et de Surete Nucleaire, Gif-sur-Yvette (France)

    1995-02-01

    The effects of humidity on the filter pressure drop have been reported in some previous studies in which it is difficult to draw definite conclusions. These studies show contradictory effects of humidity on the pressure drop probably due to differences in the hygroscopicity of the test aerosols. The objective of this paper is to present experimental results on the evolution of the filter pressure drop versus mass loading, for different test aerosols and relative humidities. Present results are compared to those found in various publication. An experimental device has been designed to measure filter pressure drop as the function of the areal density for relative humidity varying in the range of 9 % to 85 %. Experiments have been conducted with hygroscopic: (CsOH) and nonhygroscopic aerosols (TiO{sub 2}). Cesium hydroxyde (CsOH) of size of 2 {mu} M AMMD has been generated by an ultrasonic generator and the 0.7 {mu}m AMMD titanium oxyde has been dispersed by a {open_quotes}turn-table{close_quotes} generator. As it is noted in the BISWAS`publication [3], present results show, in the case of nonhygroscopic aerosols, a linear relationship of pressure drop to mass loading. For hygroscopic aerosols two cases must be considered: for relative humidity below the deliquescent point of the aerosol, the relationship of pressure drop to mass loading remains linear; above the deliquescent point, the results show a sudden increase in the pressure drop and the mass capacity of the filter is drastically reduced.

  18. Thermal infrared mapping of the Leidenfrost drop evaporation

    Science.gov (United States)

    Wciślik, Sylwia

    2016-09-01

    The paper presents an author complementary study on the Leidenfrost drop evaporation. The research was conducted under ambient conditions and in the film boiling regime. Large water drops were placed on the copper substrate of the constant temperature Tw ranging from 297.6 to 404oC. The initial single drop diameter and its mass was D0 ≈ 1cm and m0 ≈ 1g respectively. One of the obtained results, for each Tw are the drop thermal images versus time. They were used to calculate an average temperature over the drop upper surface (Td). For an exemplary heating surface temperature of Tw = 297.6oC the average drop temperature is approximately 11oC lower than the saturation one and equals Td = 88,95oC. This value is estimated for the first 200s of evaporation and with time step size Δt = 0,5s. The drop upper surface temperature is highly variable and indicates strong convection inside it. This is due to the complex nature of heat and mass transfer. The maximum standard deviation from Td = 88,95oC is SD = 1.21.

  19. Inverse Leidenfrost effect: self-propelling drops on a bath

    Science.gov (United States)

    Gauthier, Anais; van der Meer, Devaraj; Lohse, Detlef; Physics of Fluids Team

    2017-11-01

    When deposited on very hot solid, volatile drops can levitate over a cushion of vapor, in the so-called Leidenfrost state. This phenomenon can also be observed on a hot bath and similarly to the solid case, drops are very mobile due to the absence of contact with the substrate that sustains them. We discuss here a situation of ``inverse Leidenfrost effect'' where room-temperature drops levitate on a liquid nitrogen pool - the vapor is generated here by the bath sustaining the relatively hot drop. We show that the drop's movement is not random: the liquid goes across the bath in straight lines, a pattern only disrupted by elastic bouncing on the edges. In addition, the drops are initially self-propelled; first at rest, they accelerate for a few seconds and reach velocities of the order of a few cm/s, before slowing down. We investigate experimentally the parameters that affect their successive acceleration and deceleration, such as the size and nature of the drops and we discuss the origin of this pattern.

  20. Application of Proteomics to the Study of Pollination Drops

    Directory of Open Access Journals (Sweden)

    Natalie Prior

    2013-04-01

    Full Text Available Premise of the study: Pollination drops are a formative component in gymnosperm pollen-ovule interactions. Proteomics offers a direct method for the discovery of proteins associated with this early stage of sexual reproduction. Methods: Pollination drops were sampled from eight gymnosperm species: Chamaecyparis lawsoniana (Port Orford cedar, Ephedra monosperma, Ginkgo biloba, Juniperus oxycedrus (prickly juniper, Larix ×marschlinsii, Pseudotsuga menziesii (Douglas-fir, Taxus ×media, and Welwitschia mirabilis. Drops were collected by micropipette using techniques focused on preventing sample contamination. Drop proteins were separated using both gel and gel-free methods. Tandem mass spectrometric methods were used including a triple quadrupole and an Orbitrap. Results: Proteins are present in all pollination drops. Consistency in the protein complement over time was shown in L. ×marschlinsii. Representative mass spectra from W. mirabilis chitinase peptide and E. monosperma serine carboxypeptidase peptide demonstrated high quality results. We provide a summary of gymnosperm pollination drop proteins that have been discovered to date via proteomics. Discussion: Using proteomic methods, a dozen classes of proteins have been identified to date. Proteomics presents a way forward in deepening our understanding of the biological function of pollination drops.